CN110146474A - Improve CsPbCl3The method and fluorescence spectrum test method of the photoluminescence intensity of perovskite - Google Patents

Improve CsPbCl3The method and fluorescence spectrum test method of the photoluminescence intensity of perovskite Download PDF

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CN110146474A
CN110146474A CN201910372177.7A CN201910372177A CN110146474A CN 110146474 A CN110146474 A CN 110146474A CN 201910372177 A CN201910372177 A CN 201910372177A CN 110146474 A CN110146474 A CN 110146474A
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solution
cspbcl
perovskite
plasma
laser
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赵明幽
韦奕
王玉捷
史鑫宇
陈军
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material

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Abstract

The invention discloses a kind of raising CsPbCl3The method of the photoluminescence intensity of perovskite, including preparation Al@C plasma, preparation CsPbCl3Solution, by CsPbCl3Solution is mixed with Al@C plasma.Al@C plasma absorption formant and CsPbCl3Exciting light peak position is close, by utilizing its LSPR characteristic, enhances localized electromagnetic field, and the method for carrying out fluorescence spectrum test to solution using disclosed sepectrophotofluorometer, verifies CsPbCl3Solution is mixed with Al@C plasma improves CsPbCl really3Launching efficiency, realize the enhancing of PL.

Description

Improve CsPbCl3The method and fluorescence spectrum of the photoluminescence intensity of perovskite are tested Method
Technical field
The present invention relates to a kind of raising CsPbCl3The method of the photoluminescence intensity of perovskite belongs to the luminous effect of perovskite Rate technical field.
Background technique
Luminescence generated by light (Photoluminescence, abbreviation PL) is one kind of chemiluminescence, refer to material absorbing photon (or electricity Magnetic wave) after give off the process of photon (or electromagnetic wave) again.From quantum-mechanical theory, this process can be described as object Matter returns to lower state after absorbing photon transition to the excitation state of higher energy level, while discharging the process of photon.As ABX3Type calcium The CsPbCl of one of the important member of titanium ore compound3, there is luminescence generated by light effect, it, can under the exciting light irradiation of 266nm To generate the blue light of 420nm or so.Pure inorganic perovskite material, especially CsPbX3(X=Cl, Br, I) is from Kovalenko class After topic group report, because nowadays their brilliant photoelectric properties are widely regarded as new generation of semiconductor photoelectric material.System at present Standby CsPbBr3And CsPbI3The nanocrystalline PLQY (photoluminescence quantum yield) in green light and red light region reachable 90% or more, Have been widely used the gain media of active material and Low threshold Amplified Spontaneous Emission or the laser output for efficient LED.And emit CsPbX of the wavelength in blue violet light region3(X=Cl or Cl/Br) nanocrystalline luminous efficiency is low, especially CsPbCl3PLQY it is low In 10%.Mainly due to CsPbCl3Formation energy it is low, cause to generate a large amount of defects in structure, increase nonradiative transition Probability significantly limits lead halide caesium nanocrystalline material in the application in short wavelength region.Therefore, its photoluminescence efficiency is improved Seem and is even more important.
Improving the method for perovskite luminous efficiency in document at present is mainly ion doping, makes material by Doped ions Some properties are generated, such as magnetic performance, special optical performance relevant to impurity.In the nanocrystalline doping system of perovskite In, some seminars are in the nanocrystalline middle some metal ions of incorporation of lead halide caesium, such as Mn2+、Bi3+Or some rare earth ions, and This kind of doping can generate new luminous zone as caused by Doped ions, and these new luminous zones are along with from main body to doping The energy transfer of substance, this is unfavorable for the raising of host material luminous efficiency itself.
Therefore, it is necessary to a kind of raising CsPbCl3The method of the photoluminescence intensity of perovskite.
Summary of the invention
For the demand and defect of the prior art, a kind of raising CsPbCl is provided3The side of the photoluminescence intensity of perovskite Method.Its technical solution is as follows:
Step (1): Al@C plasma is prepared using liquid laser ablation.
Step 1.1: opening pulse laser, the running parameter of laser is set, when keeping laser works preheated one-section Between.
Step 1.2: reaction solution needed for configuration liquid laser ablation.Specifically includes the following steps: weighing a small amount of anti-bad Hematic acid is dissolved in toluene solution, and magneton is added and is stirred, it is ensured that it is sufficiently dissolved.
Step 1.3: installation experimental provision, main element includes Nd:YAG laser, reflecting mirror, focus lamp, double branch pipe stone English beaker, argon gas, metallic aluminium target, reaction solution.Al piece is placed in reaction solution.By adjusting optical path, so that hot spot It is directed at Al target.Laser is finally opened, adjusts voltage again, it is ensured that bombardment to the laser energy on aluminium flake is target energy, is swashed Light pulse constant bombardment is for a period of time.
Step 1.4: closing pulse laser, collect the Plasma Solutions of preparation.
Further, the running parameter in the step 1.1 include optical maser wavelength, pulse mode, pulse frequency, pulsewidth and Laser diode voltage.
Further, in step 1.3, it is passed through argon gas above reaction solution, prevents toluene solution from burning.
Further, absorption survey is carried out with Plasma Solutions of the spectrophotometer to preparation after completing step 1.4 Examination, obtains the absorption resonance peak position and CsPbCl of product3Exciting light peak position is close.
Step (2): preparation CsPbCl3Solution.
Step 2.1: by PbBr2It is dissolved in DMF solution with CsBr, and OA stirring and dissolving is added, precursor solution is made.
Step 2.2: precursor solution and poor solvent being taken to be mixed to prepare CsPbBr3Solution；
Step 2.3: by CsPbBr3Solution ultraviolet light irradiation, obtains CsPbCl3Solution.
Step 3: by CsPbCl3It is mixed in certain proportion with Al@C plasma.Simultaneously by CsPbCl3With toluene also with Same dilution proportion is as blank control group.
A method of fluorescence spectrum test being carried out for mixed solution using sepectrophotofluorometer, including is walked as follows It is rapid:
Step a: opening Fluorescence Spectrometer, connects computer and Fluorescence Spectrometer.
Step b: being put into dedicated fluid sample slot area for standard solution sample, is fixed in specimen holder.
Step c: setting parameter, including spectrum types, excitation wavelength, wavelength of transmitted light range and scanning speed.
Step d: it after the completion of parameter setting, clicks " OK " i.e. representative and is provided with.Spectrum test is carried out, screen bottom right is clicked Angle the Start Button starts emission spectrum test.
Further, after being measured, sample is taken out, cleans cuvette with toluene solution, corresponding ratio is added again Blank control group solution repeats step d and tests its emission spectrum.Two groups of solution results are compared.Use the test comparison Invention, the luminescence generated by light effect for finding out two kinds of solution of simple, intuitive.
The principle of the present invention is as follows: metal is due to being macroscopically in that electroneutral can be seen as plasma.Electricity in metal Under the irradiation of sub- Yun Guang, the variation in density can be generated due to moment electric field action, so that some region negative electrical charges are superfluous, had Region positive charge it is superfluous.The unevenness of this electron density can cause the suction of coulomb repulsion and atomic nucleus to electronics between electronics Draw, migrate electronics back and forth, shows the lengthwise oscillations of free electron density.In brief, of metal surface electron concentration Volt forms surface plasmon oscillations.When the driving frequency of light wave and the frequency of oscillation of plasma match, will occur Local surface plasma resonance (LSPR), enhances neighbouring light field.And the quantum efficiency of a centre of luminescence is Y=| L (wex)|2Z(Wem), wherein first item is to describe the intensity of local fields, it is proportional to incident field E0, and it is collected at metal Near nanostructure.So the launching efficiency of the centre of luminescence also will increase when Localized field enhancement.
The present invention is namely based on metal Al@C plasma in the LSPR effect of UV light region, the i.e. frequency of oscillation of Al@C And CsPbCl3The frequency of exciting light (ultraviolet light) matches, and local surface plasma resonance has occurred, makes CsPbCl3Particle periphery Electromagnetic enhancement, to improve CsPbCl3Launching efficiency, realize the enhancing of its PL.
Beneficial effects of the present invention:
1. CsPbCl in the present invention3It is solution with plasma, ratio regulation is convenient.
2. the present invention carries out at normal temperature, easy to operate, PL reinforcing effect is significant.
3. Al@C plasma absorption formant and CsPbCl that the present invention uses3Exciting light peak position is close, passes through utilization Its LSPR characteristic enhances localized electromagnetic field, improves CsPbCl3Launching efficiency, realize the enhancing of PL.
4: the present invention realizes CsPbCl by the way that Al@C plasma is directly added dropwise3The raising of luminous efficiency itself, avoids Since ion doping introduces new luminous zone, lead to energy transfer, is unfavorable for lacking for host material luminous efficiency raising itself Point.
Detailed description of the invention
Fig. 1 is that Al@C nano particle enhances CsPbCl3PL luminous intensity schematic diagram.
Fig. 2 is excitation state: 200-900nm, and emit state: the sepectrophotofluorometer of 200-900nm is to CsPbCl3With Al@C Nano particle 4:1 mixing and CsPbCl3The solution mixed with toluene 4:1 surveys the fluorescence spectrum of 300nm-500nm range of wavelengths Curve.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate It the present invention rather than limits the scope of the invention, after the present invention has been read, those skilled in the art are to of the invention each The modification of kind equivalent form falls within the application range as defined in the appended claims.
The method of the photoluminescence intensity of this kind of raising CsPbCl3 perovskite, includes the following steps:
Step (1): Al@C plasma is prepared using liquid laser ablation.It is specific as follows,
Step 1.1: opening pulse laser, setting optical maser wavelength is 1064nm, and adjusting laser is that Q-Switch is continuous Pulse mode, pulse frequency 10Hz, pulsewidth 10ns.Laser diode voltage is adjusted, laser energy 140mJ is made.Keep laser Work preheating 30min.
Step 1.2: reaction solution needed for configuration liquid laser ablation.Specifically includes the following steps: it is anti-bad to weigh 0.05g Hematic acid is dissolved in 30mL toluene, and magneton is added with the revolving speed of 1000r/min and stirs 10min, it is ensured that it is sufficiently dissolved.
Step 1.3: installation experimental provision, main element includes Nd:YAG laser, reflecting mirror, focus lamp, double branch pipe stone English beaker, argon gas, metallic aluminium target, reaction solution.Al piece is placed in reaction solution.Laser optical path is built, is first opened auxiliary Light is helped, so that hot spot is directed at Al target.Then it is passed through argon gas above reaction solution, prevents toluene solution from burning.Finally open Laser, adjusting voltage again makes to bombard the laser energy 140mJ on aluminium flake, and laser pulse bombards 40min.
Step 1.4: closing pulse laser, collect the Plasma Solutions of preparation.
Step 1.5: surveying 200-400nm with Plasma Solutions of the UV-3600UV-VIS-NIR spectrophotometer to preparation The absorption curve of range of wavelengths, absorption resonance peak position are 246.4nm and CsPbCl3Exciting light peak position 266nm is close.
Step 2: preparation CsPbCl3Solution.
Step 2.1: by 0.0734g PbBr2It is dissolved in 5mLDMF solution with 0.0426g CsBr, and 0.5mLOA is added Precursor solution is made in stirring and dissolving.
Step 2.2: CsPbBr can be made by taking 0.4mL precursor solution to mix with 10mL poor solvent3Solution.
Step 2.3: and then by CsPbBr3Solution ultraviolet light irradiation 3h, obtains CsPbCl3Solution.
Step 3: by CsPbCl3It is mixed with Al@C plasma with the ratio of 4:1, while by CsPbCl3With toluene also with same Sample dilution proportion is as blank control group.
Step 3.1: the preparation of standard serial solution.A clean 1.5mL centrifuge tube is taken, is added 0.10mL's in pipe After Al@C Plasma Solutions, the CsPbCl of 0.40mL is added3Solution is uniformly mixed.
Step 3.2: the preparation of blank control group solution.A clean 1.5mL centrifuge tube is taken, 0.10mL is added in pipe Toluene solution, add the CsPbCl of 0.40mL3Solution is uniformly mixed.
Step 4: carrying out fluorescence spectrum test for mixing resulting solution using sepectrophotofluorometer.
Step 4.1: opening Agilent Cary Eclipse Fluorescence Spectrometer, connect computer and Fluorescence Spectrometer.
Step 4.2: standard solution sample being put into dedicated fluid sample slot area, is fixed in specimen holder.
Step 4.3: setting spectrum types selects " Emission " emission spectrum.
Step 4.4: setting excitation wavelength.Input a length of 290.00nm of excitation light wave.
Step 4.5: setting wavelength of transmitted light range.Inputting the start wavelength of scanning and terminating wavelength is respectively 300.00nm And 500.00nm.
Step 4.6: setting scanning speed is high speed.
Step 4.7: after the completion of parameter setting, clicking " OK ".Spectrum test is carried out, the screen lower right corner " Start " is clicked and presses Button starts emission spectrum test.
Step 4.8: after being measured, taking out sample, clean cuvette with toluene solution, the sky of corresponding ratio is added again White control group solution repeats step 4.7 and tests its emission spectrum.
Test results are shown in figure 2 for two groups of solution, hence it is evident that as it can be seen that the present invention passes through in CsPbCl3Al@is introduced in solution C nano particle, based on local surface plasma resonance (LSPR) characteristic of Al@C nano particle deep ultraviolet band, by its with CsPbCl3After solution mixes in certain proportion, CsPbCl may be implemented3PL luminescence enhancement itself is to 1.5 times or so.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art The other embodiments being understood that.

Claims (7)

1. a kind of raising CsPbCl3The method of the photoluminescence intensity of perovskite, including step (1) prepare Al@C plasma, step Suddenly (2) prepare CsPbCl3Solution, it is characterised in that: step (3) is by CsPbCl3Solution is mixed with Al@C plasma.
2. raising CsPbCl according to claim 13The method of the photoluminescence intensity of perovskite, it is characterised in that: described The preparation of Al@C plasma includes the following steps:
Step 1.1: opening pulse laser, the running parameter of laser is set, laser is preheated；
Step 1.2: by dissolution of ascorbic acid in toluene solution, magneton is added and is stirred dissolution；Configuration obtains required anti- Answer solution；
Step 1.3: Al piece is placed in reaction solution；Optical path is adjusted, so that hot spot is directed at Al target；Laser is opened, is adjusted Voltage makes to bombard the laser energy target energy on aluminium flake；
Step 1.4: closing pulse laser, collect the Plasma Solutions after completing step 1.3.
3. raising CsPbCl according to claim 13The method of the photoluminescence intensity of perovskite, it is characterised in that: described CsPbCl3The preparation of solution includes:
Step 2.1: by PbBr2It is dissolved in DMF solution with CsBr, and oleic acid OA stirring and dissolving is added, precursor solution is made；
Step 2.2: precursor solution and poor solvent being taken to be mixed to prepare CsPbBr3Solution；
Step 2.3: by CsPbBr3Solution ultraviolet light irradiation, obtains CsPbCl3Solution.
4. raising CsPbCl according to claim 23The method of the photoluminescence intensity of perovskite, it is characterised in that: described Running parameter in step 1.1 includes optical maser wavelength, pulse mode, pulse frequency, pulsewidth and laser diode voltage.
5. raising CsPbCl according to claim 23The method of the photoluminescence intensity of perovskite, it is characterised in that: described In step 1.3, it is passed through argon gas above reaction solution, prevents toluene solution from burning.
6. raising CsPbCl according to claim 13The method of the photoluminescence intensity of perovskite, it is characterised in that: CsPbCl3Solution and Al@C plasma mixed proportion are 4:1.
7. a kind of method for carrying out fluorescence spectrum test to solution using sepectrophotofluorometer: it is characterized by comprising as follows Step
Step a: opening Fluorescence Spectrometer, connects computer and Fluorescence Spectrometer；
Step b: being put into fluid sample slot area for standard solution sample, is fixed in specimen holder.
Step c: setting parameter, including spectrum types, excitation wavelength, wavelength of transmitted light range and scanning speed；And it clicks and " sets Set completion " button；
Step d: carrying out spectrum test, clicks screen lower right corner START button, starts emission spectrum test.
CN201910372177.7A 2019-05-06 2019-05-06 Improve CsPbCl3The method and fluorescence spectrum test method of the photoluminescence intensity of perovskite Pending CN110146474A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110849852A (en) * 2019-11-22 2020-02-28 云南大学 Method for detecting heavy metal ions based on fluorescent perovskite nanocrystals
CN115029134A (en) * 2022-05-27 2022-09-09 广西大学 Efficient Mn-doped CsPbCl based on aluminum chloride auxiliary preparation 3 Method for producing nanocrystals

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110849852A (en) * 2019-11-22 2020-02-28 云南大学 Method for detecting heavy metal ions based on fluorescent perovskite nanocrystals
CN110849852B (en) * 2019-11-22 2020-12-22 云南大学 Method for detecting heavy metal ions based on fluorescent perovskite nanocrystals
CN115029134A (en) * 2022-05-27 2022-09-09 广西大学 Efficient Mn-doped CsPbCl based on aluminum chloride auxiliary preparation 3 Method for producing nanocrystals

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Application publication date: 20190820