CN109652060A - A kind of synthesis preparation method of organic polymer perovskite quantum dot and its application - Google Patents
A kind of synthesis preparation method of organic polymer perovskite quantum dot and its application Download PDFInfo
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Abstract
Present invention discloses a kind of synthesis preparation methods of organic polymer perovskite quantum dot, and this method comprises the following steps: S1: by CH3NH3Br, PbBr2DMF(N, dinethylformamide are dissolved in n-octyl amine) in, obtain perovskite quantum dot precursor liquid;S2: the perovskite quantum dot precursor liquid in S1 step is taken to be added in the toluene solution being vigorously stirred containing oleic acid, and keeping the volume ratio of perovskite quantum dot precursor liquid and toluene solution is 1:16 ~ 1:8, it is sufficiently stirred, reacts, obtain the perovskite quantum dot solution of clear yellow green;S3: the toluene solution of polyethylene glycol oxide is added in the perovskite quantum dot solution into S2 step, stirs, and reaction obtains polymer perovskite quantum dot solution;S4: acetonitrile reagent is added in the solution into S3 step, and centrifugation takes precipitating to dry, obtains polymer perovskite quantum dot powder.Preparation process of the present invention is simple, and the cost of raw material is cheap, easily operated.
Description
Technical field
The present invention relates to a kind of synthesis preparation method of organic polymer perovskite quantum dot and its applications, can be used for organic
Polymer chemistry synthesis technical field.
Background technique
In recent years, perovskite quantum dot is applied to light emitting diode, solar battery, laser by more and more seminars
Device, the photovoltaic arts such as optical memory, becomes the research emphasis of new energy materials field.Perovskite quantum dot has excellent light
Performance is learned, the advantages that exciton bind energy is low, carrier mobility is high, absorption spectrum is wide, glow peak is narrow is possessed, by adjusting calcium titanium
Halogen in mine quantum dot, it can be achieved that any visible light wave range luminescence generated by light.Perovskite quantum dot has the glimmering of superelevation
Quantum yield, color gamut wideness > 125% become next-generation Flexible Displays, the most potential new material of ultra-thin display.
As illuminating material, still there are various problems in actual industrial production and application in perovskite quantum dot,
In a most important problem be exactly stability problem, especially organic inorganic hybridization perovskite quantum dot.Perovskite quantum dot
To humidity, oxygen and ultraviolet light are all very sensitive, organic cation (MA+, EA+And FA+), in the effect of these environmental factors
Under easily degrade.Under usual illumination condition, perovskite surface has lone pair electrons, the organo-functional group of non-bonding and dependence
Van der Waals for is adsorbed on the organic ligand on surface, these surface defects can be with the oxygen in air, and water and carbon dioxide are anti-
It should be converted into free group, and then fallen off from perovskite surface, the reunion between perovskite quantum dot is promoted, decomposed.To have
The MA in free group and quantum dot for machine inorganic hybridization perovskite quantum dot, in solution+Reaction, which is formed, has volatility
CH3NH2, especially in the item with strong illumination (photoluminescent display devices) and strong voltage (electro-luminescence display device)
Under part, more aggravate the decomposition of perovskite quantum dot.Usual highdensity surface trap state will lead to the generation of non-radiative recombination,
It is therefore desirable to use surface capping ligand appropriate to handle the surface of perovskite quantum dot, select suitable organic poly-
It closes object to handle the surface of quantum dot, can not only reduce the surface defect of quantum dot, moreover it is possible to oxygen and moisture be inhibited to draw
The surface risen is decomposed, and the stability of perovskite quantum dot is greatly improved.
Summary of the invention
The object of the invention is to propose a kind of organic polymer calcium to solve the above-mentioned problems in the prior art
The synthesis preparation method of titanium ore quantum dot and its application.
The purpose of the invention will be achieved through the following technical solutions: kind organic polymer perovskite quantum dot synthesis
Preparation method, this method comprises the following steps:
S1: by CH3NH3Br, PbBr2It is dissolved in DMF (n,N-Dimethylformamide) with n-octyl amine, obtains perovskite amount
Son point precursor liquid;
S2: taking the perovskite quantum dot precursor liquid in S1 step to be added in the toluene solution being vigorously stirred containing oleic acid,
And keeping the volume ratio of perovskite quantum dot precursor liquid and toluene solution is 1: 16~1: 8, is sufficiently stirred, reacts, clarified
Yellow green perovskite quantum dot solution;
S3: the toluene solution of polyethylene glycol oxide is added in the perovskite quantum dot solution into S2 step, stirs, and reaction obtains
To polymer perovskite quantum dot solution;
S4: acetonitrile reagent is added in the solution into S3 step, and centrifugation takes precipitating to dry, obtains polymer perovskite quantum
Point powder.
Preferably, in the S1 step, by the CH of 0.44mmol3NH3The PbBr of Br, 0.40mmol2It is just pungent with 30 μ L
Amine is dissolved in the DMF (n,N-Dimethylformamide) of 1mL, forms transparent perovskite quantum dot precursor liquid.
Preferably, in the S2 step, contain being instilled in 0.5mL perovskite quantum dot precursor liquid obtained in S1 step
In the 8mL toluene solution being vigorously stirred for having 180 μ L oleic acid, mixed toluene solution immediately becomes yellow-green soln, owns
Reaction carries out at ambient conditions at room temperature.
Preferably, in the S3 step, by the perovskite quantum dot solution bottle obtained in S2 step after purification
It collects, is 500: 0: 500,500 according to volume ratio by perovskite Quantum Solution, the toluene solution and toluene of polyethylene glycol oxide:
125: 375,500: 250: 250,500: 375: 125,500: 500: 0, preparing sample ID respectively is A, B, C, and D and E's is organic
The toluene solution of polymer quantum dot, and be stirred at room temperature, the unit of toluene solution is 10mg mL-1。
Preferably, in the S4 step, after polyethylene glycol oxide and perovskite quantum dot solution encapsulation reaction are complete, to
Appropriate acetonitrile reagent is added dropwise in the toluene of organic polymer quantum dot will be yellow after 4500rpm. centrifugation 10min is arranged in centrifuge speed
The precipitating of color is dried, and obtains organic polymer perovskite quantum dot powder.
Preferably, the structure of the organic polymer perovskite quantum dot is ABX3, wherein A is that methylamine, carbonamidine, caesium are organic
Or pure inorganic cation, B are lead, copper, germanium metallic element, X is chlorine, bromine, iodine halogen;A be methylamine, carbonamidine, caesium it is a kind of or
Two or more organic or pure inorganic cation.
Preferably, in the S3 step, the molecular weight of polyethylene glycol oxide is 200-1000000.
Preferably, the polyethylene glycol oxide is other ionic conductance polymerizations prepared based on the polymer.
Preferably, the organic polymer perovskite quantum dot solution, solvent are that toluene, chlorobenzene, n-hexane, acetonitrile can
It dissolves quantum dot and does not destroy the weak polar solvent of its structure.
Present invention further teaches a kind of application of organic polymer perovskite quantum dot, the organic polymer perovskite amount
Son point can be applied to solar battery, light emitting diode, laser, thin film transistor (TFT), photodetector or micro sensing device.
The invention adopts the above technical scheme compared with prior art, has following technical effect that this method using water-soluble
Property polymer polyoxyethylene carries out mixing package to it, and the addition of polyethylene glycol oxide plays perovskite quantum dot surface blunt
The effect for changing encapsulation, reduces the surface defect of perovskite quantum dot, the oxygen and moisture reduced in air causes perovskite
The decomposition of quantum dot surface, it is suppressed that non-radiative recombination caused by the defect state of perovskite quantum dot surface, the calcium titanium after package
The fluorescence quantum efficiency of mine quantum dot improves 59%.Solve current perovskite quantum dot, especially organic inorganic hybridization perovskite
Quantum dot surface defect is more, the problem of stability difference.In addition, preparation process of the present invention is simple, the cost of raw material is cheap, repeatability
Height, it is easily operated, it is light emitting diode, optical detector, solar battery, the optics device such as devices such as photodetector and micro sensing
Part field provides effective active layer material preparation method.
Detailed description of the invention
Fig. 1 is the preparation flow figure of Inventive polymers perovskite quantum dot solution.
Fig. 2 is the transmission electron microscope picture of Inventive polymers perovskite quantum dot.
Fig. 3 is the Fourier infrared absorption figure of Inventive polymers perovskite quantum dot.
Fig. 4 is the X-ray photoelectron spectroscopic analysis figure of Inventive polymers perovskite quantum dot.
Fig. 5 is the decay life time figure of Inventive polymers perovskite quantum dot;
Specific embodiment
The purpose of the present invention, advantage and feature, by by the non-limitative illustration of preferred embodiment below carry out diagram and
It explains.These embodiments are only the prominent examples using technical solution of the present invention, it is all take equivalent replacement or equivalent transformation and
The technical solution of formation, all falls within the scope of protection of present invention.
Present invention discloses a kind of synthesis preparation method of organic polymer perovskite quantum dot, this method includes following step
It is rapid:
S1: by CH3NH3Br, PbBr2It is dissolved in DMF (n,N-Dimethylformamide) with n-octyl amine, obtains perovskite amount
Son point precursor liquid;
S2: taking the perovskite quantum dot precursor liquid in S1 step to be added in the toluene solution being vigorously stirred containing oleic acid,
And keeping the volume ratio of perovskite quantum dot precursor liquid and toluene solution is 1: 16~1: 8, is sufficiently stirred, reacts, clarified
Yellow green perovskite quantum dot solution;
S3: the toluene solution of polyethylene glycol oxide is added in the perovskite quantum dot solution into S2 step, stirs, and reaction obtains
To polymer perovskite quantum dot solution;
S4: acetonitrile reagent is added in the solution into S3 step, and centrifugation takes precipitating to dry, obtains polymer perovskite quantum
Point powder.
In the S1 step, by the CH of 0.44mmol3NH3The PbBr of Br, 0.40mmol2It is dissolved with the n-octyl amine of 30 μ L
In the DMF (n,N-Dimethylformamide) of 1mL, transparent perovskite quantum dot precursor liquid is formed.
In the S2 step, contain 180 μ L for instilling in 0.5mL perovskite quantum dot precursor liquid obtained in S1 step
In the 8mL toluene solution of oleic acid being vigorously stirred, mixed toluene solution immediately becomes yellow-green soln, and all reactions exist
It carries out at ambient conditions at room temperature.
In the S3 step, the perovskite quantum dot solution obtained in S2 step after purification is collected with bottle, it will
The toluene solution and toluene of perovskite Quantum Solution, polyethylene glycol oxide are 500: 0: 500,500: 125: 375 according to volume ratio,
500: 250: 250,500: 375: 125,500: 500: 0, preparing sample ID respectively is A, B, C, the organic polymer object amount of D and E
The toluene solution of son point, and be stirred at room temperature, the unit of toluene solution is 10mg mL-1。
In the S4 step, after polyethylene glycol oxide and perovskite quantum dot solution encapsulation reaction are complete, gather to organic
Appropriate acetonitrile reagent is added dropwise in the toluene for closing object quantum dot, after 4500rpm. centrifugation 10min is arranged in centrifuge speed, by the heavy of yellow
Shallow lake is dried, and obtains organic polymer perovskite quantum dot powder.
The structure of the organic polymer perovskite quantum dot is ABX3, wherein A be methylamine, carbonamidine, caesium etc. it is organic or
Pure inorganic cation, B are lead, copper, and the metallic elements such as germanium, X is chlorine, bromine, the halogens such as iodine.
In the S3 step, the molecular weight of polyethylene glycol oxide is 200-1000000.The polyethylene glycol oxide is poly- with this
Close other ionic conductance polymerizations prepared based on object.The organic polymer perovskite quantum dot solution, solvent be toluene,
Chlorobenzene, n-hexane, acetonitrile can be such that quantum dot dissolves and not destroy the weak polar solvent of its structure.
The perovskite quantum dot that this method is prepared, can be applied to solar battery, light emitting diode, laser, film
Transistor, photodetector or micro sensing device.
Embodiment 1
The process that is synthetically prepared of perovskite organic polymer quantum dot of the present invention specifically includes the following steps:
(1) synthesis of perovskite quantum dot
By the CH of 0.44mmol3NH3Br (methyl bromide ammonium), the PbBr of 0.40mmol2The n-octyl amine of (lead bromide) and 30 μ L
It is dissolved in the DMF (n,N-Dimethylformamide) of 1mL, forms transparent transparent precursor solution.Then, by 0.5mL forerunner
Liquid solution instills in the 8mL toluene solution being vigorously stirred containing 180 μ L oleic acid.At this point, mixed toluene solution becomes immediately
For yellow-green soln.All reactions carry out at 21.5 DEG C of room temperature at ambient conditions.
(2) preparation of organic polymer quantum dot
Perovskite quantum dot solution after purification is collected with bottle with bottle, by perovskite Quantum Solution, polyoxyethylene
The toluene solution and toluene of alkene are 500: 0: 500,500: 125: 375,500: 250: 250,500: 375: 125 according to volume ratio,
500: 500: 0, preparing sample ID respectively is A, B, C, the toluene solution of the organic polymer quantum dot of D and E, and at room temperature
Stirring, the unit of toluene solution are 10mg mL-1。
(3) preparation of organic polymer quantum dot powder
After polyethylene glycol oxide and perovskite quantum dot encapsulation reaction are complete, it is added dropwise to the toluene of organic polymer quantum dot
Appropriate acetonitrile the precipitating of yellow is dried, as organic polymer after 4500rpm. centrifugation 10min is arranged in centrifuge speed
Object quantum dot powder.
Fig. 1 is the preparation flow figure of polymer perovskite quantum dot in the invention.The high performance calcium that the present embodiment is obtained
Titanium ore organic polymer quantum dot is characterized.
Fig. 2 is the transmission electron microscope picture of polymer perovskite quantum dot.Use polymer according to the present invention
The dispersibility that the toluene solvant of perovskite quantum dot has had prepared by the preparation method of perovskite quantum dot, perovskite quantum
The structure of point is without because the addition of polyethylene glycol oxide changes.
Fig. 3 is the Fourier infrared absorption figure of polymer perovskite quantum dot.Use polymer calcium according to the present invention
Perovskite quantum dot prepared by the preparation method of titanium ore quantum dot, does not change quantum-dot structure feature.Do not use polyoxy
Change N-H the vibration peak (~3010cm of the perovskite quantum dot surface of ethylene processing-1And 732cm-1), O-H vibration peak (~939cm-1), C=O vibration peak (~1713cm-1), C-H vibration peak (~3010cm-1And 732cm-1) relatively strong;But these vibration peaks with
The increase of polyoxyethylene content, which gradually weakens, even to disappear, also, stretches peak C O (~1110cm-1) key gradually increases, it shows
Appear in 838cm-1, 958cm-1, 1643cm-1, 1243cm-1, 1289cm-1, 1345cm-1And 1360cm-1Place occurs bright
- CH in aobvious polyethylene glycol oxide2Vibration peak illustrates that perovskite quantum dot is wrapped up by polyethylene glycol oxide.
Fig. 4 is the X-ray photoelectron spectroscopic analysis figure of polymer perovskite quantum dot.Use polymerization according to the present invention
Perovskite quantum dot prepared by the preparation method of object perovskite quantum dot, does not change quantum-dot structure feature, with polyoxy
Change the increase of ethylene contents, C the and O peak intensity of perovskite quantum dot all increases sharply, and Br, Pb and the peak N do not become significantly
Change, illustrate that perovskite quantum is wrapped up by polyethylene glycol oxide, and to change the functional group inside quantum dot.
Fig. 5 is the decay life time figure of polymer perovskite quantum dot.Use polymer calcium titanium according to the present invention
The average life span of perovskite quantum dot prepared by the preparation method of mine quantum dot obviously increases, and the defect state ratio on surface is in calcium
Ratio in titanium ore quantum dot reduces.
This method is for solving current perovskite quantum, especially organic inorganic hybridization perovskite quantum dot surface defect
It is more, the problem of stability difference.The present invention carries out mixing package to perovskite quantum dot using water-soluble polymer polyethylene glycol oxide
The addition of processing, polyethylene glycol oxide plays the role of passivation encapsulation to perovskite quantum dot surface, reduces perovskite quantum
The surface defect of point, reduces the decomposition that oxygen and moisture in air cause perovskite quantum dot surface, it is suppressed that perovskite
Non-radiative recombination caused by the defect state of quantum dot surface, the fluorescent quantum effect of the organic polymer perovskite quantum dot after package
Rate improves 59%.Preparation process of the present invention is simple, and the cost of raw material is cheap, and repeatability is high, easily operated, is light emitting diode,
The optical devices such as devices such as optical detector, solar battery, photodetector and micro sensing field provides effective active layer
Material preparation method.
Still there are many embodiment, all technical sides formed using equivalents or equivalent transformation by the present invention
Case is within the scope of the present invention.
Claims (10)
1. a kind of synthesis preparation method of organic polymer perovskite quantum dot, it is characterised in that: this method comprises the following steps:
S1: by CH3NH3Br, PbBr2It is dissolved in DMF (n,N-Dimethylformamide) with n-octyl amine, obtains perovskite quantum dot
Precursor liquid;
S2: it takes the perovskite quantum dot precursor liquid in S1 step to be added in the toluene solution being vigorously stirred containing oleic acid, and protects
The volume ratio for holding perovskite quantum dot precursor liquid and toluene solution is 1: 16~1: 8, is sufficiently stirred, reacts, obtain clear Huang
The perovskite quantum dot solution of green;
S3: the toluene solution of polyethylene glycol oxide is added in the perovskite quantum dot solution into S2 step, stirs, and reaction is gathered
Close object perovskite quantum dot solution;
S4: acetonitrile reagent is added in the solution into S3 step, and centrifugation takes precipitating to dry, obtains polymer perovskite quantum dot powder
End.
2. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 1, it is characterised in that:
In the S1 step, by the CH of 0.44mmol3NH3The PbBr of Br, 0.40mmol2It is dissolved in 1mL's with the n-octyl amine of 30 μ L
In DMF (n,N-Dimethylformamide), transparent perovskite quantum dot precursor liquid is formed.
3. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 2, it is characterised in that:
In the S2 step, the play containing 180 μ L oleic acid will be instilled in 0.5mL perovskite quantum dot precursor liquid obtained in S1 step
In the 8mL toluene solution of strong stirring, mixed toluene solution immediately becomes yellow-green soln, and all reactions exist at room temperature
It is carried out under environmental condition.
4. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 3, it is characterised in that:
In the S3 step, the perovskite quantum dot solution obtained in S2 step after purification is collected with bottle, by perovskite amount
The toluene solution and toluene of sub- solution, polyethylene glycol oxide are 500: 0: 500,500: 125: 375,500: 250 according to volume ratio:
250,500: 375: 125,500: 500: 0, preparing sample ID respectively is A, B, C, the first of the organic polymer quantum dot of D and E
Benzole soln, and be stirred at room temperature, the unit of toluene solution is 10mg mL-1。
5. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 4, it is characterised in that:
In the S4 step, after polyethylene glycol oxide and perovskite quantum dot solution encapsulation reaction are complete, to organic polymer quantum
The toluene of point is added dropwise appropriate acetonitrile reagent and does the precipitating of yellow after 4500rpm. centrifugation 10min is arranged in centrifuge speed
It is dry, obtain organic polymer perovskite quantum dot powder.
6. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 5, it is characterised in that:
The structure of the organic polymer perovskite quantum dot is ABX3, wherein A be that methylamine, carbonamidine, caesium be organic or pure inorganic sun from
Son, B are lead, copper, germanium metallic element, and X is chlorine, bromine, iodine halogen;A be methylamine, carbonamidine, caesium it is one or two kinds of above organic or
The pure inorganic cation of person.
7. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 1, it is characterised in that:
In the S3 step, the molecular weight of polyethylene glycol oxide is 200-1000000.
8. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 7, it is characterised in that:
The polyethylene glycol oxide is other ionic conductance polymerizations prepared based on the polymer.
9. a kind of synthesis preparation method of organic polymer perovskite quantum dot according to claim 5, it is characterised in that:
The organic polymer perovskite quantum dot solution, solvent be toluene, chlorobenzene, n-hexane, acetonitrile can make quantum dot dissolve and
The weak polar solvent of its structure is not destroyed.
10. a kind of application of organic polymer perovskite quantum dot, it is characterised in that: the organic polymer perovskite quantum dot
It can be applied to solar battery, light emitting diode, laser, thin film transistor (TFT), photodetector or micro sensing device.
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