CN111760537B - Apparatus and method for synthesizing perovskite-type material - Google Patents

Apparatus and method for synthesizing perovskite-type material Download PDF

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CN111760537B
CN111760537B CN202010500309.2A CN202010500309A CN111760537B CN 111760537 B CN111760537 B CN 111760537B CN 202010500309 A CN202010500309 A CN 202010500309A CN 111760537 B CN111760537 B CN 111760537B
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perovskite
type material
reaction
synthesizing
injection pump
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CN111760537A (en
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徐曜
朱熹
陆一骅
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Shenzhen Institute of Artificial Intelligence and Robotics
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Shenzhen Institute of Artificial Intelligence and Robotics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1862Stationary reactors having moving elements inside placed in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/02Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C01G21/006Compounds containing, besides lead, two or more other elements, with the exception of oxygen or hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The present invention relates to a device and a method for synthesizing a perovskite-type material. The apparatus for synthesizing the perovskite-type material includes: the reaction mechanism comprises a first reaction container, a first heating stirrer, a second reaction container and a second heating stirrer; the solid adding mechanism comprises an injection piston and a pushing piece, the injection piston can bear solid powder, and the pushing piece can push the injection piston to move so as to add the solid powder into the first reaction container; the liquid adding mechanism comprises a vessel, a first injection pump and a second injection pump; the control mechanism is used for controlling the temperature and the rotating speed of the first heating stirrer and the second heating stirrer and controlling the movement of the pushing piece and the flow rates of the first injection pump and the second injection pump. The synthesis device for the perovskite type material can automatically synthesize the perovskite type material, and has high synthesis efficiency and high operation accuracy.

Description

Apparatus and method for synthesizing perovskite-type material
Technical Field
The invention relates to the field of materials, in particular to a device and a method for synthesizing a perovskite type material.
Background
With the continuous development of chemical experimental technology and the application of intellectualization to various industries, the improvement of experimental work efficiency has become a necessary and social consensus. Various devices are developing towards the direction of being convenient to install, simple to operate, space-saving, safe, efficient, intelligent, automatic and the like. Due to the special structure of the perovskite material, the perovskite material has potential application prospect in the aspects of high-temperature catalysis and photocatalysis. The traditional perovskite type material synthesis is relatively complex in weighing and other operations, has certain deviation, and simultaneously needs personnel to operate, and has the problem of low efficiency in synthesis.
Disclosure of Invention
In view of this, it is necessary to provide a perovskite-type material synthesis apparatus capable of automatically synthesizing a perovskite-type material with high synthesis efficiency and high operation accuracy.
In addition, a method for synthesizing the perovskite type material is also provided.
An apparatus for synthesizing a perovskite-type material, comprising:
the reaction mechanism comprises a first reaction vessel, a first heating stirrer for heating the first reaction vessel, a second reaction vessel and a second heating stirrer for heating the second reaction vessel, and the first reaction vessel and the second reaction vessel can both contain reaction reagents;
the solid adding mechanism comprises an injection piston and a pushing piece, the injection piston can contain solid powder, and the pushing piece can push the injection piston to move so as to add the solid powder into the first reaction vessel;
the liquid adding mechanism comprises a vessel for containing a liquid sample, a first injection pump and a second injection pump, wherein the first injection pump is used for adding the liquid sample in the vessel into the first reaction container, and the second injection pump is used for adding a reaction reagent in the first reaction container into the second reaction container; and
a control mechanism for controlling the temperature and rotational speed of the first and second heated agitators and for controlling the movement of the pusher, the infusion flow rates of the first and second infusion pumps.
In one embodiment, the injection device further comprises a housing, the first heating stirrer and the first reaction container are arranged inside the housing, the housing is provided with a top plate, the top plate is provided with a sample inlet, the injection piston and the pushing member are both arranged on the top plate, and the injection piston, the first injection pump and the second injection pump are all communicated with the first reaction container through the sample inlet.
In one embodiment, the second heated agitator, the second reaction vessel, the first syringe pump, and the second syringe pump are all disposed outside the housing.
In one embodiment, the pusher is a lead screw guide.
In one embodiment, the control mechanism includes a computer and a single chip microcomputer, the computer is connected with the single chip microcomputer through a serial port, the computer is further connected with the first heating stirrer, the second heating stirrer, the first injection pump and the second injection pump through serial ports so as to control the first heating stirrer, the second heating stirrer, the first injection pump and the second injection pump through the serial ports, the single chip microcomputer is electrically connected with the pushing member, and the single chip microcomputer can control the movement of the pushing member so as to enable the pushing member to push the injection piston to move.
In one embodiment, the single chip microcomputer comprises an STM32 control plate, and the STM32 control plate is electrically connected with the pushing piece.
In one embodiment, the liquid adding mechanism further comprises a plurality of connecting pipes for communicating the vessel, the first syringe pump and the first reaction vessel and communicating the first reaction vessel, the second syringe pump and the second reaction vessel.
In one embodiment, there are two of the vessels, the first syringe pump is in communication with one of the vessels, and the liquid addition mechanism further comprises a third syringe pump in communication with the other of the vessels.
A method for synthesizing a perovskite-type material using the apparatus for synthesizing a perovskite-type material, comprising the steps of:
adding a polar solvent into the first reaction container, adding a non-polar solvent into the second reaction container, adding solid powder into the injection piston, and adding a stabilizing agent into the container;
the control mechanism controls the first injection pump to add a fixed amount of stabilizing agent into the first reaction container, the control mechanism controls the pushing piece to drive the injection piston to move, and a fixed amount of solid powder is added into the first reaction container;
controlling the temperature and the rotating speed of the first heating stirrer through the control mechanism, observing the state of the reaction liquid in the first reaction vessel, and controlling the second injection pump to quantitatively add the reaction liquid in the first reaction vessel into the second reaction vessel through the control mechanism when the reaction liquid is clear; and
and controlling the temperature and the rotating speed of the second heating stirrer through the control mechanism to enable the liquid in the second reaction vessel to react to prepare the perovskite type material.
In one embodiment, the solid powder comprises a first halide and a second halide, the first halide being CH3NH3X、HC(NH2)2X or CsX, the second halide being PbX2Or SnX2Wherein, X is chlorine, bromine or iodine.
In one embodiment, the first halide is cesium bromide, the second halide is lead bromide, and the molar ratio of the first halide to the second halide is 1:3 to 1: 6.
In one embodiment, the polar solvent is selected from at least one of N, N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methylpyrrolidone; the nonpolar solvent is selected from at least one of o-xylene, toluene and chloroform.
In one embodiment, the stabilizer is selected from at least one of oleic acid and oleylamine.
Above-mentioned synthesizer of perovskite type material can be through the injection piston, the impeller, cooperation between control mechanism and the first heating agitator, realize the automation and the accurate joining of solid powder, through first syringe pump, second syringe pump and control mechanism's cooperation, realize that liquid sample is automatic and the accurate joining, weigh when avoiding manual operation and the error of volume, the quality of the perovskite type material that the accuracy and preparation obtained has been improved, through control mechanism, the cooperation of first heating agitator and second heating agitator, realize the control of process parameter in the reaction process, therefore synthesizer of above-mentioned perovskite type material can the auto-synthesis perovskite type material, the synthesis efficiency is improved. Therefore, the above-described synthesis apparatus has advantages of automatic synthesis of perovskite-type materials, high synthesis efficiency, and high operation accuracy.
Drawings
FIG. 1 is a schematic structural view of an apparatus for synthesizing a perovskite-type material according to an embodiment;
FIG. 2 is a schematic view showing the connection between a control mechanism and other mechanisms in the apparatus for synthesizing a perovskite-type material shown in FIG. 1;
fig. 3 is a process flow diagram of a method for synthesizing a perovskite-type material according to an embodiment.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Element number description:
a perovskite-type material synthesizing device 10; the reaction mechanism 100: a first reaction vessel 110, a first heating stirrer 120, a second reaction vessel 130, a second heating stirrer 140; solid adding mechanism 200: the injection piston 210, the pusher 220; liquid addition mechanism 300: a vessel 310, a first syringe pump 320, a second syringe pump 330, a third syringe pump 340, a connecting pipe 350; the control mechanism 400: a computer 410, a single chip 420; the housing 500: top plate 510, sample inlet 520.
Referring to fig. 1, an embodiment of an apparatus 10 for synthesizing a perovskite-type material includes: a reaction mechanism 100, a solid adding mechanism 200, a liquid adding mechanism 300, and a control mechanism 400.
The reaction mechanism 100 includes a first reaction vessel 110, a first heating stirrer 120 for heating the first reaction vessel 110, a second reaction vessel 130, and a second heating stirrer 140 for heating the second reaction vessel 130, the first reaction vessel 110 being capable of housing a reaction reagent, and the second reaction vessel 130 being capable of housing a reaction reagent.
Specifically, in the present embodiment, the first heating stirrer 120 and the second heating stirrer 140 are both magnetic heating stirrers. It is understood that in other embodiments, the first heating stirrer 120 and the second heating stirrer 140 may be other conventional devices having heating and stirring functions. The first heating stirrer 120 can control the reaction temperature and the stirring speed of the reaction liquid in the first reaction vessel 110. The second heating stirrer 140 can control the temperature and stirring speed of the reaction liquid within the second reaction vessel 130.
Wherein the first reaction vessel 110 can contain a polar solvent. The polar solvent is at least one selected from the group consisting of N, N-dimethylformamide, dimethyl sulfoxide, tetrahydrofuran and N-methylpyrrolidone. The second reaction vessel 130 can contain a non-polar solvent. The nonpolar solvent is selected from at least one of o-xylene, toluene and chloroform. It is to be understood that the polar solvent and the nonpolar solvent are not limited to the above, and may be polar solvents and nonpolar solvents commonly used in the art for preparing perovskite-type materials, or may be adjusted according to the structure and properties of the prepared perovskite-type materials.
Referring to fig. 2, the solid adding mechanism 200 includes an injection piston 210 and a pushing member 220, the injection piston 210 can contain solid powder, and the pushing member 220 can push the injection piston 210 to move so as to add the solid powder into the first reaction vessel 110. In particular, the injection piston 210 is connected with a pusher 220.
In one embodiment, the pusher 220 is a lead screw rail. When the pushing member 220 is a lead screw guide rail, the structure of the pushing member 220 may be a structure commonly used in the art, for example, the pushing member 220 includes a lead screw, a guide rail, a slider, a motor, and the like, the lead screw can push the slider to move in the guide rail under the driving of the motor, and the slider is connected with the injection piston 210. The pushing member 220 can push the injection piston 210 to move, and thus, the automatic addition of the solid powder into the first reaction vessel 110 is realized.
The solid powder includes a first halide and a second halide. The first halide being CH3NH3X、HC(NH2)2X or CsX, the second halide being PbX2Or SnX2Wherein, X is chlorine, bromine or iodine. In one embodiment, the solid powder is a mixture of lead bromide and cesium bromide, and the molar ratio of the lead bromide to the cesium bromide in the solid powder is 1: 3-1: 6. When the first halide is cesium bromide and the second halide is lead bromide in the above molar ratio, Cs can be produced4PbBr6A zero-dimensional perovskite nanocrystal. It is to be understood that in other embodiments, the first halide and the second halide may be other substances, and the molar ratio of the first halide and the second halide is not limited to the above value, and may be adjusted according to the structure of the perovskite-type material to be prepared.
The liquid adding mechanism 300 includes a vessel 310 for containing a liquid sample, a first syringe pump 320, and a second syringe pump 330, the first syringe pump 320 is used for adding the liquid sample in the vessel 310 into the first reaction vessel 110, and the second syringe pump 330 is used for adding the reaction liquid in the first reaction vessel 110 into the second reaction vessel 130.
Specifically, vessel 310 is used to house a stabilizer. The stabilizer is at least one selected from oleic acid and oleylamine. In one embodiment, the stabilizer comprises oleic acid and oleylamine. The composite stabilizer of oleic acid and oleylamine can improve the solubility of the raw materials, thereby realizing the efficient utilization of the reaction raw materials.
When the stabilizer comprises oleic acid and oleylamine, the vessel 310 may contain a mixture of oleic acid and oleylamine mixed in a certain ratio. In addition, the number of the vessels 310 may be two, wherein one vessel 310 is used for containing the oleic acid, and the other vessel 310 is used for containing the oleylamine. The first syringe pump 320 is in communication with one of the vessels 310, and the liquid addition mechanism 300 further includes a third syringe pump 340, the third syringe pump 340 being in communication with the other vessel 310. By setting the two vessels 310, the dosages of the oleic acid and the oleylamine can be independently controlled by the first syringe pump 320 and the third syringe pump 340, and the dosages of the oleic acid and the oleylamine can be flexibly adjusted.
In one embodiment, vessel 310 is a beaker. It is understood that in other embodiments, the vessel 310 is not limited to a beaker, but may be a container capable of holding a liquid sample, such as a flask, a conical flask, etc., commonly used in the art.
Specifically, the liquid adding mechanism 300 further includes a plurality of connection pipes 350, the plurality of connection pipes 350 respectively communicate the first vessel 310, the first syringe pump 320 and the first reaction container 110, and communicate the first reaction container 110, the second syringe pump 330 and the second reaction container 130, and the plurality of connection pipes 350 also communicate the second vessel 310, the third syringe pump 340 and the first reaction container 110. In one embodiment, the connection tube 350 is a hose. The hose has better flexibility, no blockage and no stiffness; the weight is light, and the caliber consistency is good; the flexibility, repeated bending property and flexibility are good; corrosion resistance and the like, and can be suitable for various liquid samples. It is understood that in other embodiments, the connection pipe 330 is not limited to a hose, but may be other conventional pipes.
In one embodiment, the first syringe pump 320, the second syringe pump 330, and the third syringe pump 340 are all industrial syringe pumps. It is understood that in other embodiments, the first syringe pump 320, the second syringe pump 330, and the third syringe pump 340 can be other commonly used pumps.
The control mechanism 400 is used to control the temperature and rotational speed of the first and second heated mixers 120, 140 and to control the movement of the pusher 220 and the injection flow rates of the first and second syringe pumps 320, 330. Specifically, when the liquid adding mechanism 300 further includes the third syringe pump 340, the control mechanism is also used to control the flow rate of the third syringe pump 340. Specifically, the control mechanism 400 is connected to the first heating stirrer 120, the second heating stirrer 140, the pushing member 220, the first injection pump 320 and the second injection pump 330 through serial ports.
In one embodiment, referring to fig. 2, the control mechanism 400 includes a computer 410 and a single chip 420, wherein the computer 410 is connected to the first heating stirrer 120, the second heating stirrer 140, the first syringe pump 320 and the second syringe pump 330 through serial ports, so as to control the first heating stirrer 120, the second heating stirrer 140, the first syringe pump 320 and the second syringe pump 330 through the serial ports. The computer 410 can control the heating temperature and the stirring speed of the first and second heated mixers 120 and 140, and the computer 410 can control the on/off and flow rate of the first, second and third syringe pumps 320, 330 and 340.
The single chip 420 is connected with the computer 410 through a serial port, and the single chip 420 is also electrically connected with the pushing member 220. The single chip 420 is used for controlling the movement of the pushing member 220 so that the pushing member 220 pushes the injection piston 210 to move, and the injection piston 210 adds the solid powder into the first reaction vessel 110. Specifically, the single chip 420 controls the motor of the pushing member 220 to work, so that the pushing member 220 is controlled to move, and the automatic feeding of the solid powder is realized. In one embodiment, the single chip 420 includes an STM32 control board. Further, the single chip microcomputer 420 is an STM32 control panel. The STM32 control plate is electrically connected to the pusher member 220. The STM32 control panel can accurately control the motion of impeller, realizes the accurate interpolation of solid sample to weighing error when reducing personnel's operation.
Further, the first heating agitator 120 also has a weighing function capable of weighing the mass of the solid powder added to the first reaction vessel 110, and the first heating agitator 120 is also capable of feeding back the mass to the control mechanism 400, and the control mechanism 400 is capable of controlling the movement of the pushing member 220 in accordance with the mass fed back by the first heating agitator 120. Specifically, the first heated agitator 120 can feed back the mass to the computer 410 of the control mechanism 400, and the computer 410 of the control mechanism 400 can control the movement of the pusher member 220 based on the mass fed back by the first heated agitator 120. In actual use, the mass of the solid powder to be added is input into the computer 410, and then the pushing member 220 is controlled by the single chip 420 to move so as to push the injection piston 210 to add the solid powder into the first reaction vessel 110. When the mass of the solid powder added reaches a preset value, the computer 410 controls the single chip 420 such that the pushing member 220 does not move any more, thereby stopping the injection piston 210 from adding the solid powder into the first reaction vessel 110. Through the combined action of the first heating stirrer 120, the injection piston 210, the pushing member 220, the single chip microcomputer 420 and the computer 410, the dosage of the added solid powder can be accurately controlled, and the problems of operation errors of manual weighing and low efficiency are avoided.
Specifically, the above-described perovskite-type material synthesis apparatus 10 further includes a housing 500. The first heating stirrer 120 and the first reaction vessel 110 are disposed inside the case 500, and the second heating stirrer 140 and the second reaction vessel 130 are disposed outside the case 500. When the first heating stirrer 120 and the second heating stirrer 140 are both magnetic heating stirrers, in order to avoid magnetic field interference between the two heating stirrers, the first heating stirrer 120 and the second heating stirrer 140 are respectively arranged inside and outside the housing 500, so as to ensure accuracy of results.
The vessel 310, the first syringe pump 320, the second syringe pump 330, and the third syringe pump 340 are all disposed outside the housing 500. The vessel 310, the first syringe pump 320, the second syringe pump 330 and the third syringe pump 340 are disposed outside the housing 500, so that the liquid can be conveniently injected at any time, and the synthesis reaction can be continuously performed. In addition, the computer 410 of the control mechanism 400 is also disposed outside the housing 500 to facilitate operation of the computer 410 to control operation of other mechanisms.
Specifically, the housing 500 is provided with a top plate 510, and the injection piston 210 and the pusher 220 are both disposed on the top plate 510 of the housing 500. Specifically, the injection piston 210 and the pusher 220 are fixed to the top plate of the housing 500. The top plate 510 is also provided with a sample inlet 520. The injection piston 210, the first injection pump 320, the second injection pump 330 and the third injection pump 340 are all communicated with the first reaction vessel 110 through the sample inlet 520. Specifically, the first syringe pump 320, the second syringe pump 330, and the third syringe pump 340 are communicated with the sample inlet 520 through the connection tube 350, and the connection tube 350 can pass through the sample inlet 520. Specifically, there are two sample inlets 520, and one sample inlet 520 is a liquid inlet and is communicated with the first syringe pump 320, the second syringe pump 330, and the third syringe pump 340 through the connection tube 350. The other sample inlet 520 is a solid sample inlet and is in communication with the injection piston 210. The sample inlets 520 are two, so that the sample introduction of the solid powder and the liquid sample is facilitated.
By providing the housing 500, on the one hand, the precursor reaction can be performed inside the housing 500, and interference by other substances can be avoided, and on the other hand, the solid adding mechanism 200 can be provided on the top plate 510 of the housing 500, and the structure can be more compact and simpler.
In one embodiment, the housing 500 is an aluminum alloy housing.
The working principle of the perovskite type material is as follows: the computer 410 is connected with the single chip 420 through an electric line to realize communication control, the single chip 420 is electrically connected with the pushing member 220, the single chip 420 controls the pushing member 220 to do linear reciprocating motion, the pushing member 220 does linear reciprocating motion to push the injection piston 210 to add solid powder into the first reaction vessel 110, and the accurate quantitative addition of the solid powder is realized through the control of the first heating stirrer 120 and the computer 410. The computer 410 is connected with the first injection pump 320, the second injection pump 330 and the third injection pump 340 through serial ports to control the flow rate of the liquid passing through the first injection pump 320, the second injection pump 330 and the third injection pump 340, thereby realizing the quantitative addition of the liquid sample. The computer 410 is connected to the first heating stirrer 120 and the second heating stirrer 140 via serial ports to control the stirring speed and temperature of the first heating stirrer 120 and the second heating stirrer 140, so as to control the process parameters during the reaction process.
The perovskite-type material synthesizing apparatus 10 has at least the following advantages:
(1) the synthesis device 10 for perovskite type materials can realize automatic synthesis of perovskite type materials, avoids the complexity, low efficiency and the like of manual operation, and improves the synthesis efficiency.
(2) The synthesis device 10 for perovskite type materials can realize the accurate control of the dosage of solid powder through the matching among the injection piston 210, the pushing piece 220, the single chip microcomputer and the first heating stirrer 120, realize the accurate control of the dosage of liquid powder through the matching of the first injection pump 320, the second injection pump 330, the third injection pump 340 and the computer 410, avoid the errors of weighing and dosage during manual operation, and improve the accuracy and the quality of the prepared perovskite type materials.
Referring to fig. 3, a method for synthesizing a perovskite-type material according to an embodiment includes the following steps:
step S110: provided is a device for synthesizing a perovskite-type material.
The synthesizing device in step S110 is the synthesizing device for the perovskite-type material according to the above embodiment, and is not described herein again.
Step S120: adding polar solvent into the first reaction container, adding non-polar solvent into the second reaction container, adding solid powder into the injection piston, and adding stabilizer into the container.
Wherein the polar solvent is at least one selected from N, N-dimethylformamide, dimethyl sulfoxide, tetrahydrofuran and N-methylpyrrolidone. The nonpolar solvent is selected from at least one of o-xylene, toluene and chloroform. It is to be understood that the polar solvent and the non-polar solvent are not limited to the above-mentioned ones, and may be polar solvents and non-polar solvents commonly used in the art.
Specifically, the solid powder comprises a first halide and a second halide, the first halide being CH3NH3X、HC(NH2)2X or CsX, the second halide being PbX2Or SnX2Wherein, X is chlorine, bromine or iodine.
In one embodiment, the solid powder is a mixture of lead bromide and cesium bromide, and the molar ratio of the lead bromide to the cesium bromide in the solid powder is 1: 3-1: 6. When the first halide is cesium bromide and the second halide is lead bromide in the above molar ratio, Cs can be produced4PbBr6A zero-dimensional perovskite nanocrystal. It is to be understood that in other embodiments, the first halide and the second halide may be other substances, and the molar ratio of the first halide and the second halide is not limited to the above value, and may be adjusted according to the structure of the perovskite-type material to be prepared.
The stabilizer is at least one selected from oleic acid and oleylamine. In one embodiment, the stabilizer comprises oleic acid and oleylamine. The composite stabilizer of oleic acid and oleylamine can improve the solubility of the raw materials, thereby realizing the efficient utilization of the reaction raw materials.
Step S130: the control mechanism controls the first injection pump to add quantitative stabilizing agent into the first reaction container, and the control mechanism controls the pushing piece to drive the injection piston to move, so that quantitative solid powder is added into the first reaction container.
Specifically, a preset amount of the stabilizer to be added is given at the computer, and then the first syringe pump is controlled to add the preset amount of the stabilizer to the first reaction vessel. Through computer control, first syringe pump carries out, has realized the accurate control of stabilizer quantity, has solved the problem that the operational error and the operating efficiency are low of stabilizer are got to manual volume.
Through the motion of singlechip control impeller to promote the motion of injection piston, add solid powder in to first reaction vessel, combine the mass weighing in the first heating agitator simultaneously, the error of artifical weighing has been avoided to the quantity of the solid powder of accurate control joining, has realized the automation and the accuracy of solid powder and has added.
Step S140: the temperature and the rotating speed of the first heating stirrer are controlled by the control mechanism, the state of the reaction liquid in the first reaction vessel is observed, and when the reaction liquid is clear, the third injection pump is controlled by the control mechanism to add the reaction liquid in the first reaction vessel into the second reaction vessel.
In the first reaction vessel, the solid powder is dissolved in a polar solvent to obtain a precursor solution. In one embodiment, the first heated agitator has a temperature of 60 ℃ and a rotational speed of 700 r/min. It will be appreciated that in other embodiments, the temperature and rotational speed of the first heated stirrer are not limited to the values described above, but may be adjusted as is conventional in the art, or otherwise, depending on the structure and properties of the perovskite-type material to be produced.
Step S150: the temperature and the rotating speed of the second heating stirrer are controlled by the control mechanism, so that the liquid in the second reaction vessel is subjected to mixing reaction to prepare the perovskite type material.
Specifically, the temperature of the second heating stirrer is room temperature, and the rotating speed is 500 r/min. It will also be appreciated that in other embodiments, the temperature and rotational speed of the second heated agitator are not limited to the values described above, but may be other parameters commonly used in the art, or may be adjusted depending on the structure and properties of the perovskite-type material to be produced.
The synthesis method of the perovskite type material at least has the following advantages:
(1) the synthesis method of the perovskite type material realizes the automatic synthesis of the perovskite type material, improves the synthesis efficiency of the perovskite type material, and can be applied to the large-scale production of the perovskite type material.
(2) The synthesis method of the perovskite type material can accurately control the dosage of each added substance, and avoids errors in the manual operation process, so that the synthesized perovskite type material has better performance and high consistency.
The following are specific examples:
example 1
The perovskite-type material of the present embodiment is specifically synthesized as follows:
(1) 2g of the mixed powder (1: 5 molar ratio of lead bromide to cesium bromide) was added in advance to the solid injection piston, sufficient oleic acid was added to the first vessel, sufficient oleylamine was added to the second vessel, and 15mL of N, N-dimethylformamide was added to the first reaction vessel and 50mL of o-xylene was added to the second reaction vessel.
(2) The first injection pump and the third injection pump are controlled by a computer to respectively add 1mL of oleic acid and 1mL of oleylamine into the first reaction vessel, and the screw guide rail is controlled by the computer to move so as to push the injection piston to add 0.5g of solid powder into the first reaction vessel.
(3) The temperature of the first heating stirrer is controlled by a computer to be 60 ℃ and the rotating speed is controlled to be 700 r/min. When the solution in the first reaction vessel became clear, 1mL of the reacted precursor solution in the first reaction vessel 110 was pumped into the second reaction vessel by the second syringe pump.
(4) By using a meterAnd controlling the rotating speed of the second heating stirrer to be 500r/min by the computer so as to enable the liquid in the second reaction vessel to react. Reacting for 2 minutes to obtain Cs4PbBr6Perovskite nanocrystals.
The above examples enable Cs to be obtained4PbBr6The perovskite nanocrystalline has high operation efficiency, and the synthesized perovskite nanocrystalline has good quality and excellent performance.
It should be noted that only Cs is shown in the above examples4PbBr6The process for synthesizing perovskite nanocrystals, and the process for synthesizing other perovskite-type materials, are similar to those of example 1, and are not described herein again.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (12)

1. A method for synthesizing a perovskite-type material, characterized by synthesizing the perovskite-type material using a perovskite-type material synthesizing apparatus comprising:
the reaction mechanism comprises a first reaction container, a first heating stirrer for heating the first reaction container, a second reaction container and a second heating stirrer for heating the second reaction container, and the first reaction container and the second reaction container can both contain reaction reagents;
the solid adding mechanism comprises an injection piston and a pushing piece, the injection piston can contain solid powder, and the pushing piece can push the injection piston to move so as to add the solid powder into the first reaction vessel;
the liquid adding mechanism comprises a vessel for containing a liquid sample, a first injection pump and a second injection pump, wherein the first injection pump is used for adding the liquid sample in the vessel into the first reaction container, and the second injection pump is used for adding a reaction reagent in the first reaction container into the second reaction container; and
a control mechanism for controlling the temperature and rotational speed of the first and second heated mixers and for controlling the movement of the pusher, the infusion flow rates of the first and second infusion pumps;
the synthesis method comprises the following steps:
adding a polar solvent into the first reaction container, adding a non-polar solvent into the second reaction container, adding solid powder into the injection piston, and adding a stabilizing agent into the container;
the control mechanism controls the first injection pump to add a fixed amount of stabilizing agent into the first reaction container, the control mechanism controls the pushing piece to drive the injection piston to move, and a fixed amount of solid powder is added into the first reaction container;
controlling the temperature and the rotating speed of the first heating stirrer through the control mechanism, observing the state of the reaction liquid in the first reaction vessel, and controlling the second injection pump to quantitatively add the reaction liquid in the first reaction vessel into the second reaction vessel through the control mechanism when the reaction liquid is clear; and
the temperature and the rotating speed of the second heating stirrer are controlled by the control mechanism, so that the liquid in the second reaction vessel reacts to prepare the perovskite type material.
2. The method for synthesizing a perovskite-type material according to claim 1, wherein the synthesizing apparatus further comprises a housing, the first heating stirrer and the first reaction vessel are disposed inside the housing, the housing is provided with a top plate, the top plate is provided with a sample inlet, the injection piston and the pushing member are disposed on the top plate, and the injection piston, the first injection pump and the second injection pump are all communicated with the first reaction vessel through the sample inlet.
3. The method for synthesizing a perovskite-type material according to claim 2, wherein the second heating stirrer, the second reaction vessel, the first injection pump and the second injection pump are disposed outside the casing.
4. The method of synthesizing a perovskite-type material of claim 1, wherein the pusher is a lead screw rail.
5. The method for synthesizing a perovskite-type material according to claim 1, wherein the control mechanism comprises a computer and a single chip microcomputer, the computer is connected with the single chip microcomputer through a serial port, the computer is further connected with the first heating stirrer, the second heating stirrer, the first injection pump and the second injection pump through serial ports so as to control the first heating stirrer, the second heating stirrer, the first injection pump and the second injection pump through serial ports, the single chip microcomputer is electrically connected with the pushing member, and the single chip microcomputer can control the movement of the pushing member so as to enable the pushing member to push the injection piston to move.
6. The method of synthesizing a perovskite-type material as claimed in claim 5, wherein the monolithic processor comprises a STM32 control board, the STM32 control board being electrically connected to the pusher member.
7. The method for synthesizing a perovskite-type material according to claim 1, wherein the liquid addition mechanism further comprises a plurality of connection pipes for communicating the vessel, the first syringe pump and the first reaction vessel with each other and for communicating the first reaction vessel, the second syringe pump and the second reaction vessel with each other.
8. The method of synthesizing a perovskite-type material as claimed in claim 1, wherein there are two of said vessels, said first syringe pump being in communication with one of said vessels, said liquid addition mechanism further comprising a third syringe pump in communication with the other of said vessels.
9. The method for synthesizing a perovskite-type material as claimed in any one of claims 1 to 8, wherein the solid powder comprises a first halide and a second halide, and the first halide is CH3NH3X、HC(NH22X or CsX, the second halide being PbX2Or SnX2Wherein, X is chlorine, bromine or iodine.
10. The method for synthesizing a perovskite-type material according to claim 9, wherein the first halide is cesium bromide, the second halide is lead bromide, and a molar ratio of the first halide to the second halide is 1:3 to 1: 6.
11. The method for synthesizing a perovskite-type material according to claim 1, wherein the polar solvent is at least one selected from the group consisting of N, N-dimethylformamide, dimethylsulfoxide, tetrahydrofuran, and N-methylpyrrolidone; the nonpolar solvent is selected from at least one of o-xylene, toluene and chloroform.
12. The method for synthesizing a perovskite-type material according to claim 1, wherein the stabilizer is at least one selected from oleic acid and oleylamine.
CN202010500309.2A 2020-06-04 2020-06-04 Apparatus and method for synthesizing perovskite-type material Expired - Fee Related CN111760537B (en)

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CN204320137U (en) * 2014-12-11 2015-05-13 江西格力特水产饲料有限公司 A kind of aquatic feeds mixing arrangement
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