CN108393049A - A kind of low temperature process efficiently prepares the micro-reaction device and method of blue light perovskite quantum dot - Google Patents

A kind of low temperature process efficiently prepares the micro-reaction device and method of blue light perovskite quantum dot Download PDF

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Publication number
CN108393049A
CN108393049A CN201810340902.8A CN201810340902A CN108393049A CN 108393049 A CN108393049 A CN 108393049A CN 201810340902 A CN201810340902 A CN 201810340902A CN 108393049 A CN108393049 A CN 108393049A
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quantum dot
blue light
microchannel
channel
perovskite quantum
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李宗涛
汤勇
余彬海
卢汉光
饶龙石
宋存江
陆龙生
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South China University of Technology SCUT
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South China University of Technology SCUT
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Priority to CN201810340902.8A priority Critical patent/CN108393049A/en
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Priority to PCT/CN2018/111937 priority patent/WO2019200876A1/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • C09K11/664—Halogenides
    • C09K11/665—Halogenides with alkali or alkaline earth metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00018—Construction aspects
    • B01J2219/0002—Plants assembled from modules joined together
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00353—Pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction

Abstract

A kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, including syringe pump, reactor, temperature control module；Temperature control module includes temperature controller, water-cooling head, thermostatic water bath；Reactor includes upper cover plate and microchannel, and the lower section of upper cover plate is fixed in microchannel；Syringe pump is set to the top of reactor, and temperature controller is installed on the center on the surface of upper cover plate and is electrically connected with microchannel, and water-cooling head is tightly attached to microchannel lower surface, and is coated with one layer of heat-conducting silicone grease on the contact surface, and water-cooling head is connected with thermostatic water bath by water pipe；The upper surface of microchannel be equipped be sequentially connected it is logical take part in Taoism, first passage, second channel, third channel, fourth lane.A kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, and the micro-reaction device of blue light perovskite quantum dot is efficiently prepared using a kind of low temperature process.The present invention has the advantages that good mixing effect, high integration, preparation efficiency is high.The invention belongs to technical field of photoelectric material preparation.

Description

A kind of low temperature process efficiently prepares the micro-reaction device and method of blue light perovskite quantum dot
Technical field
The invention belongs to technical field of photoelectric material preparation, and in particular to a kind of low temperature process efficiently prepares blue light perovskite amount The micro-reaction device and method of son point.
Background technology
LED illumination and display product are due to luminous efficiency height, and energy saving, colour rendering is good, long lifespan, one since birth Directly by the extensive concern of society.The most of structure for using P-N junction of LED product currently on the market, uses the knot of P-N junction The disadvantages such as that there is emission peaks is wider for the product of structure, and fluorescence efficiency is low, cause LED product light efficiency colour rendering index relatively low, not yet Achieve the effect that people are expected.And the halide perovskite quantum dot having gradually developed in recent years, have emission peak relatively narrow, it is glimmering The advantages that light efficiency may be up to 90%, and launch wavelength is adjustable, the QLED devices prepared on its basis, can preferably improve colour temperature, The properties such as the logical, light efficiency of light, there is huge application value.But current perovskite quantum dot technology of preparing is also very immature, it is special It is not combination problem of the perovskite quantum dot due to Cl ions and matrix of blue light, more than not in fluorescence quantum efficiency etc. Upper green light perovskite quantum dot；In addition existing preparation method uses traditional reaction unit, and efficiency is too low, it is difficult to disposably make Standby a large amount of perovskite quantum dot, finds a kind of blue light perovskite quantum dot preparation method of continuous high-efficient, has great grind Study carefully value.
Invention content
In view of the above-mentioned problems, the present invention provides micro- reaction dress that a kind of low temperature process efficiently prepares blue light perovskite quantum dot It sets, it has the advantages that good mixing effect, high integration, preparation efficiency is high, prepared blue light perovskite quantum dot fluorescence effect Rate is high, and the regulation and control of wavelength are continuously accurate.
It is a further object of the present invention to provide micro- reaction methods that a kind of low temperature process efficiently prepares blue light perovskite quantum dot.
A kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, it is characterised in that：Including syringe pump, Reactor, temperature control module；
Temperature control module includes temperature controller, water-cooling head, thermostatic water bath；
Reactor includes upper cover plate and microchannel, and the lower section of upper cover plate is fixed in microchannel；
Syringe pump is set to the top of reactor, and temperature controller is installed on the center on the surface of upper cover plate and is electrically connected with microchannel It connects, water-cooling head is tightly attached to microchannel lower surface, and one layer of heat-conducting silicone grease, water are coated on the contact surface of water-cooling head and microchannel Cold head is connected with thermostatic water bath by water pipe；
The upper surface of microchannel be equipped be sequentially connected it is logical take part in Taoism, first passage, second channel, third channel, four-way Road, first passage, second channel, third channel, fourth lane are the microchannel of one group of ring-buckling type, pass through pipe between each channel Road is connected, and the microchannel of every group of ring-buckling type includes being sequentially connected logical multiple annulus microchannels, is in ring between annulus microchannel Ring interlocks connection, upper equipped with first entrance, second entrance taking part in Taoism, and third is equipped in the junction of second channel and third channel Entrance is equipped with product exit in the end of fourth lane.
Preferably, the microchannel of every group of ring-buckling type includes being sequentially connected four logical annulus microchannels, and annulus microchannel is Dislocation type microchannel, a ring are narrow channel, and another ring is wide type channel, and the dislocation distance in wide type channel and narrow channel is 0.4mm-0.6mm, wide type channel are arc-shaped, and the radian in wide type channel is 90 ° -150 °.
Preferably, narrow channel caliber is 0.4mm-0.6mm, and wide type channel caliber is 0.9mm-1.2mm,
Preferably, take part in Taoism including it is main take part in Taoism, first takes part in Taoism and takes part in Taoism with second, first take part in Taoism with second take part in Taoism merging become owner of into Road, main take part in Taoism are connected with the first circulation passage；First, which takes part in Taoism, is equipped with first entrance, and second, which takes part in Taoism, is equipped with second entrance；The The caliber of pipeline between one channel, second channel, third channel, fourth lane is 1.5mm-2mm.
Preferably, microchannel is made of semiconductor chilling plate, on the huyashi-chuuka (cold chinese-style noodles) of semiconductor chilling plate processing channel, spray again Apply one layer of boron nitride.
Upper cover plate is made of aluminum alloy material.
A kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, efficient using a kind of above-mentioned low temperature process The micro-reaction device for preparing blue light perovskite quantum dot, includes the following steps：
(1) device assembles：A kind of low temperature process is efficiently prepared to the micro-reaction device assembling of blue light perovskite quantum dot；
(2) mixed solution is configured：Oleyl amine and oleic acid are measured, puts DMF solvent into, is stirred with the rotating speed of 900-1200r/min Dissolving, DMF solvent, oleic acid, oleyl amine volume ratio be 20:2:1；
(3) it is equipped with DMF-PbBr2Solution and DMF-CsBr solution：Weigh PbBr respectively on electronic balance2Solid and CsBr Solid, and PbBr2The molar ratio of solid and CsBr solids is 2:1, and it is molten to be added separately to the mixing configured in two parts of steps (2) It in liquid, then is stirred evenly with the rotating speed of 900-1200r/min, respectively obtains DMF-PbBr2Solution and DMF-CsBr solution；
(4) temperature control module is set：The switch of thermostatic water bath and temperature controller is opened, the water temperature of thermostatic water bath is set as 5 DEG C -10 DEG C, the water flow of thermostatic water bath is set as 1.5L/min-2.5L/min, and temperature controller target temperature value is set as -50 DEG C -0 DEG C；
(5) transferring raw material：Wait for that actual temperature reaches set target temperature value, respectively from first entrance and second entrance with equal Even rate is passed through DMF-PbBr2Solution and DMF-CsBr solution are passed through toluene from third entrance with uniform rate；
(6) collection of products：The blue light perovskite quantum dot generated is collected in product exit.
Preferably, first entrance is passed through DMF-PbBr2The rate and second entrance of solution are passed through the speed of DMF-CsBr solution Rate is 0.5mL/min-1.5mL/min, and the rate that third entrance is passed through toluene is 5-10mL/min.
Preferably, DMF-PbBr2The concentration of solution and DMF-CsBr solution is 0.2mmoL/mL-0.4mmoL/mL.
Preferably, in step (2), oleyl amine 1mL, oleic acid 0.5mL, DMF solvent 10mL.
Preferably, PbBr is weighed2Solid 0.147g and CsBr solid 0.043g.
Advantages of the present invention：
1, microchannel integrated level height, each channel size are smaller in the present invention, utilize the Peltier effect of semiconductor chilling plate Preferable refrigeration effect is obtained, in the raw material PbBr of green light perovskite quantum dot2On the basis of CsBr, by control temperature with Perovskite quantum point grain diameter is controlled, using the principle of supersaturation crystallization to which high-efficiency and continuous synthesizes blue light perovskite quantum dot, Good mixing effect, integrated level is high, and preparation efficiency is high.
2, annulus microchannel composition all linked with one another is all made of in the present invention using four channels, and each annulus is micro- logical Road is all made of dislocation type microchannel, the distance dislocation in the wide type channel and narrow channel and caliber of the two is small, therefore microchannel collection It is more preferable at degree higher, mixed effect, prepare that blue light perovskite quantum dot is at low cost, output is high.
3, operating procedure of the present invention is simple, and prepared blue light perovskite quantum dot wavelength is in 430nm- in the present invention 487nm accurately regulates and controls, and for half-peak breadth between 29-33nm, fluorescence quantum yield is high far above previous traditional blue light carbon quantum dot Up to 85% or more, the blue light perovskite quantum dot of preparation can be used for the necks such as light emitting diode, LED light emitting device and LED display Domain, therefore the blue light perovskite quantum dot effect prepared is good, has a wide range of application.
Description of the drawings
Fig. 1 is a kind of combination diagram of the micro-reaction device of low temperature preparation blue light perovskite quantum dot.
Fig. 2 is the structural schematic diagram of reactor in the present invention；
Fig. 3 is the structural schematic diagram of microchannel in the present invention；
Fig. 4 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 1.
Fig. 5 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 2.
Fig. 6 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 3.
Fig. 7 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 4.
Fig. 8 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 5.
Fig. 9 is the launching light spectrogram of the blue light perovskite quantum dot obtained by embodiment 6.
Wherein, 1- first entrances, 2- second entrances, 3- third entrances, 4- product exits, 5- presoma production districts, before 6- Drive body and toluene mixed zone, 7- fasteners, 8- upper cover plates, the microchannels 9-, 10- syringe pumps, 11- reactors, 12- temperature control modules, 13- temperature controllers, 14- water-cooling heads, 15- thermostatic water baths.
Specific implementation mode
The present invention is further illustrated below in conjunction with the accompanying drawings.
Embodiment one：
A kind of micro-reaction device of low temperature preparation blue light perovskite quantum dot, including syringe pump, reactor and temperature control module, Syringe pump is set to the top of reactor, and temperature control module is connected with reactor.Temperature control module includes temperature controller, water-cooling head, thermostatted water Slot.
Such as Fig. 1, upper cover plate is made of aluminum alloy material, and temperature controller is mounted on the center of upper cover plate, and temperature controller is thermoelectricity It is even；The microchannel that semiconductor chilling plate is process is electrically connected with temperature controller；Water-cooling head is close to the lower surface of microchannel, and in water Coated on cold head and the contact surface of microchannel thickness 0.2mm-0.3mm heat-conducting silicone grease；Water-cooling head is with thermostatic water bath with water pipe It is connected.
As shown in Fig. 2, reactor includes microchannel, upper cover plate；Microchannel is fixed on the lower section of upper cover plate by fastener. Fastener is made of screw bolt and nut.
As shown in figure 3, microchannel is made of semiconductor chilling plate, and processing channel on the huyashi-chuuka (cold chinese-style noodles) of semiconductor chilling plate, One layer of boron nitride coating is sprayed again to be formed.Channel on the huyashi-chuuka (cold chinese-style noodles) of microchannel include be sequentially connected connect take part in Taoism, first passage, Two channels, third channel, fourth lane；First passage, second channel, third channel, fourth lane are one group of ring-buckling type Microchannel is connected by pipeline between each channel；The microchannel of every group of ring-buckling type is by being in ring ring phase by four annulus microchannels Button connection composition.Each annulus microchannel in group is dislocation type microchannel, and a ring is narrow channel, and another ring is that wide type is logical Road, narrow channel caliber are 0.4mm-0.6mm, and wide type channel caliber is 0.9mm-1.2mm, the mistake in wide type channel and narrow channel Position distance is 0.4mm-0.6mm, and wide type channel is arc-shaped, and the radian in wide type channel is 90 ° -150 °, namely wide type channel The angle that misplaces is 90 ° -150 °.The caliber of connecting pipe between first passage, second channel, third channel, fourth lane is 1.5mm-2mm.Take part in Taoism including it is main take part in Taoism, first takes part in Taoism and takes part in Taoism with second, first, which takes part in Taoism, becomes owner of and takes part in Taoism with the second merging of taking part in Taoism, main It takes part in Taoism and is connected with the first circulation passage.First, which takes part in Taoism, is equipped with first entrance, and second, which takes part in Taoism, is equipped with second entrance.It is logical second The junction of road and third channel is equipped with third entrance；The end of fourth lane is equipped with product exit.
Take part in Taoism, first passage, second channel constitute presoma generation area, third channel, fourth lane constitute presoma with Toluene mixed zone.
A kind of micro- reaction method that low temperature process efficiently prepares blue light perovskite quantum dot specifically includes in the present embodiment Following steps：
(1) a kind of micro-reaction device of low temperature preparation blue light perovskite quantum dot is assembled；In the present embodiment, (a) will Reactor group installs, and the connection caliber between each channel is set as 1.5mm, and each annulus microchannel in group is logical for dislocation type Road, half are narrow channel, the other half is wide type channel, and narrow channel caliber is 0.5mm, and wide type channel caliber is 1.0mm, wide The dislocation distance in type channel is 0.5mm, and the radian in wide type channel is 120 °；(b) connect reactor and temperature control module, water-cooling head with The contact surface of microchannel coats the heat-conducting silicone grease that thickness is 0.3mm.
(2) oleic acid for measuring the oleyl amine and 0.5mL of 1mL, puts 10mL DMF solvents (dimethylformamide) into, and with The rotating speed stirring and dissolving of 900r/min.
(3) 0.147g PbBr are weighed respectively on electronic balance2With 0.043g CsBr solid (molar ratios 2:1), and It is added separately in two parts of obtained mixed solutions of step (2), and is stirred evenly with the rotating speed of 900r/min, respectively obtained DMF-PbBr2Solution and DMF-CsBr solution.
(4) switch of thermostatic water bath and temperature controller is opened, the water temperature of thermostatic water bath is set as 5 DEG C, and water flow is set as 2.5L/ Min, temperature controller target temperature value are set as 0 DEG C.
(5) wait for that actual temperature reaches set 0 DEG C of target temperature value, respectively from the first entrance of reactor and second entrance with The rate of 1mL/min is passed through DMF-PbBr2Solution and DMF-CsBr solution are passed through first from third entrance with the rate of 5mL/min Benzene obtains blue light perovskite quantum dot from the collection of product exit.
Such as the launching light spectrogram that Fig. 4 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 487nm, half-peak breadth 33nm.
Abscissa in Fig. 4 to Fig. 9 is wavelength X, and the unit of wavelength is nm, and ordinate is fluorescence intensity A, and fluorescence is strong The unit of degree is a.u..
Embodiment two：
The present embodiment and embodiment one the difference is that temperature controller target temperature value is set as -10 DEG C in step (4), other Condition remains unchanged；Something in common is repeated no more.
Such as the launching light spectrogram that Fig. 5 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 465nm, half-peak breadth 32nm.
According to document (CsPbX3Quantum Dots for Lighting and Displays:Room‐ Temperature Synthesis,Photoluminescence Superiorities,Underlying Origins and White Light‐Emitting Diodes[J].Advanced Functional Materials,2016,26(15): Method 2435-2445) reported uses flask as reaction vessel under popular response system, utilizes PbBr2、CsBr、 PbCl2And CsCl, blue light perovskite quantum dot is made and measures fluorescence volume using quinine sulfate as reference according to reference method step Sub- efficiency is 64%.
PbBr is used under micro-reaction device according to embodiment two2With blue light perovskite quantum dot made from CsBr, according to Reference method step, it is 88% that fluorescence quantum efficiency is measured using quinine sulfate as reference.
Embodiment three：
The present embodiment and embodiment one the difference is that temperature controller target temperature value is set as -20 DEG C in step (4), other Condition remains unchanged；Something in common is repeated no more.
Such as the launching light spectrogram that Fig. 6 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 448nm, half-peak breadth 30nm.
Example IV：
The present embodiment and embodiment one the difference is that temperature controller target temperature value is set as -30 DEG C in step (4), other Condition remains unchanged；Something in common is repeated no more.
Such as the launching light spectrogram that Fig. 7 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 437nm, half-peak breadth 29nm.
Embodiment five：
The present embodiment and embodiment one the difference is that temperature controller target temperature value is set as -40 DEG C in step (4), other Condition remains unchanged；Something in common is repeated no more.
Such as the launching light spectrogram that Fig. 8 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 430nm, half-peak breadth 32nm.
Embodiment six：
The present embodiment and embodiment one the difference is that temperature controller target temperature value is set as -50 DEG C in step (4), other Condition remains unchanged；Something in common is repeated no more.
Such as the launching light spectrogram that Fig. 9 is blue light perovskite quantum dot manufactured in the present embodiment, as seen from the figure, obtained quantum Point launch wavelength is 430nm, half-peak breadth 31nm.
Above-described embodiment is to invent preferable embodiment, but embodiments of the present invention are not limited by above-described embodiment System, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications, Equivalent substitute mode is should be, is included within the scope of the present invention.

Claims (10)

1. a kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, it is characterised in that：Including syringe pump, instead Answer device, temperature control module；
Temperature control module includes temperature controller, water-cooling head, thermostatic water bath；
Reactor includes upper cover plate and microchannel, and the lower section of upper cover plate is fixed in microchannel；
Syringe pump is set to the top of reactor, and temperature controller is installed on the center on the surface of upper cover plate and is electrically connected with microchannel, water Cold head is tightly attached to microchannel lower surface, and one layer of heat-conducting silicone grease, water-cooling head are coated on the contact surface of water-cooling head and microchannel It is connected by water pipe with thermostatic water bath；
The upper surface of microchannel be equipped be sequentially connected it is logical take part in Taoism, first passage, second channel, third channel, fourth lane, the One channel, second channel, third channel, fourth lane are the microchannel of one group of ring-buckling type, pass through pipeline phase between each channel Connection, the microchannel of every group of ring-buckling type includes being sequentially connected logical multiple annulus microchannels, is in ring ring phase between annulus microchannel Button connection, it is upper equipped with first entrance, second entrance taking part in Taoism, enter equipped with third in the junction of second channel and third channel Mouthful, it is equipped with product exit in the end of fourth lane.
2. a kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, feature according to claim 1 It is：The microchannel of every group of ring-buckling type includes being sequentially connected four logical annulus microchannels, and annulus microchannel is that dislocation type is micro- logical Road, a ring are narrow channel, and another ring is wide type channel, and the dislocation distance in wide type channel and narrow channel is 0.4mm-0.6mm, Wide type channel is arc-shaped, and the radian in wide type channel is 90 ° -150 °.
3. a kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, feature according to claim 2 It is：Narrow channel caliber is 0.4mm-0.6mm, and wide type channel caliber is 0.9mm-1.2mm.
4. a kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, feature according to claim 1 It is：Take part in Taoism including it is main take part in Taoism, first takes part in Taoism and takes part in Taoism with second, first, which takes part in Taoism, becomes owner of and takes part in Taoism with the second merging of taking part in Taoism, and master takes part in Taoism It is connected with the first circulation passage；First, which takes part in Taoism, is equipped with first entrance, and second, which takes part in Taoism, is equipped with second entrance；First passage, The caliber of pipeline between two channels, third channel, fourth lane is 1.5mm-2mm.
5. a kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, feature according to claim 1 It is：Microchannel is made of semiconductor chilling plate, on the huyashi-chuuka (cold chinese-style noodles) of semiconductor chilling plate processing channel, spray one layer of nitridation again Boron.
6. a kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, any described using claim 1-5 A kind of low temperature process efficiently prepares the micro-reaction device of blue light perovskite quantum dot, it is characterised in that：
(1) device assembles：A kind of low temperature process is efficiently prepared to the micro-reaction device assembling of blue light perovskite quantum dot；
(2) mixed solution is configured：Oleyl amine and oleic acid are measured, puts DMF solvent into, with the rotating speed stirring and dissolving of 900-1200r/min, DMF solvent, oleic acid, oleyl amine volume ratio be 20:2:1；
(3) it is equipped with DMF-PbBr2Solution and DMF-CsBr solution：Weigh PbBr respectively on electronic balance2Solid and CsBr are solid Body, and PbBr2The molar ratio of solid and CsBr solids is 2:1, and it is added separately to the mixed solution configured in two parts of steps (2) In, then stirred evenly with the rotating speed of 900-1200r/min, respectively obtain DMF-PbBr2Solution and DMF-CsBr solution；
(4) temperature control module is set：The switch of thermostatic water bath and temperature controller is opened, the water temperature of thermostatic water bath is set as 5 DEG C -10 DEG C, perseverance The water flow of warm water tank is set as 1.5L/min-2.5L/min, and temperature controller target temperature value is set as -50 DEG C -0 DEG C；
(5) transferring raw material：Wait for that actual temperature reaches set target temperature value, respectively from first entrance and second entrance with uniform Rate is passed through DMF-PbBr2Solution and DMF-CsBr solution are passed through toluene from third entrance with uniform rate；
(6) collection of products：The blue light perovskite quantum dot generated is collected in product exit.
7. a kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, feature according to claim 6 It is：First entrance is passed through DMF-PbBr2The rate that the rate and second entrance of solution are passed through DMF-CsBr solution is 0.5mL/min-1.5mL/min, the rate that third entrance is passed through toluene are 5-10mL/min.
8. a kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, feature according to claim 6 It is：DMF-PbBr2The concentration of solution and DMF-CsBr solution is 0.2mmoL/mL-0.4mmoL/mL.
9. a kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot, feature according to claim 6 It is：In step (2), oleyl amine 1mL, oleic acid 0.5mL, DMF solvent 10mL.
10. a kind of low temperature process efficiently prepares micro- reaction method of blue light perovskite quantum dot its feature according to claim 6 It is：Weigh DMF-PbBr2Solid 0.147g and CsBr solid 0.043g.
CN201810340902.8A 2018-04-17 2018-04-17 A kind of low temperature process efficiently prepares the micro-reaction device and method of blue light perovskite quantum dot Pending CN108393049A (en)

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CN201810340902.8A CN108393049A (en) 2018-04-17 2018-04-17 A kind of low temperature process efficiently prepares the micro-reaction device and method of blue light perovskite quantum dot
PCT/CN2018/111937 WO2019200876A1 (en) 2018-04-17 2018-10-25 Micro-reaction device and method for efficiently preparing blue light perovskite quantum dots by means of low temperature method

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