CN115141628A - Preparation method of lead-free halide double perovskite nanocrystalline - Google Patents
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Abstract
The application discloses a preparation method of a lead-free halide double perovskite nanocrystal, which comprises the following steps; (S100) obtaining a solution L1 of a precursor CsX; (S200) obtaining a solution L2 containing AgY, MZ and hydrogen halide; (S300) adding the solution L1 into the solution L2, mixing, reacting, and cooling to obtain the lead-free halide double perovskite nano crystal. The nanocrystalline prepared by the preparation method has uniform components and uniform size, the luminous efficiency is obviously improved, and the adjustment of the spectrum and the conversion of the luminous color are realized.
Description
Technical Field
The application relates to a preparation method of a lead-free halide double perovskite nanocrystal, belonging to the field of perovskite nanocrystals.
Background
The lead halide perovskite nano crystal has the advantages of wide luminescent color gamut, easy regulation and control of spectrum in a visible light range, narrow half-peak width, high fluorescence quantum yield and the like, so that the lead halide perovskite nano crystal has great potential in the fields of solar cells, light-emitting diodes, photocatalysis and the like. However, lead is toxic, harmful to the human body, and sensitive to water and oxygen, which limits its commercial application. The search for non-toxic and stable perovskite materials becomes a current research hotspot.
The all-inorganic lead-free halide double perovskite nano crystal is free of toxic elements, environment-friendly, harmless to human bodies, excellent in water-oxygen stability and expected to replace lead-free halide perovskites. In the aspect of research on environment-friendly perovskite nanocrystals, lead-free double-halide perovskites are undoubtedly a better choice.
At present, a plurality of results are obtained through research on a plurality of lead-free halide double perovskite nanocrystals, but the problem of low quantum yield of the lead-free halide double perovskite nanocrystals is always to be solved urgently, so that a method for remarkably improving the quantum yield of the lead-free halide double perovskite nanocrystals is urgently needed at present.
Disclosure of Invention
Aiming at the problem of low quantum yield of the existing lead-free halide double perovskite nano crystal, a novel preparation method is provided, the preparation method is prepared by a thermal injection method which is simple in component optimization and convenient to use, the quantum yield can be obviously improved, and the optical performance of the material is improved.
According to a first aspect of the present application, a method for preparing a lead halide-free double perovskite nanocrystal is provided.
A preparation method of lead-free halide double perovskite nanocrystal comprises the following steps;
(S100) obtaining a solution L1 of a precursor CsX;
(S200) obtaining a solution L2 containing AgY, MZ and hydrogen halide;
(S300) adding the solution L1 into the solution L2, reacting, and cooling to obtain the lead-free halide double perovskite nano-crystal;
wherein X is selected from CO 3 2- At least one of halogen anion;
m is selected from Bi and/or In;
y and Z are independently selected from at least one of halide anions.
Optionally, the halide anion comprises Cl - 、Br - 、I - 。
Alternatively, csX is selected from Cs 2 CO 3 At least one of CsCl, csBr and CsI.
Optionally, agY is selected from at least one of AgCl, agBr, agI.
Alternatively, MZ is selected from BiCl 3 、BiBr 3 、BiI 3 、InCl 3 、InBr 3 、InI 3 At least one of (1).
Alternatively, the hydrogen halide is selected from at least one of HCl, HBr, HI.
Alternatively, the molar ratio of AgY, MZ and hydrogen halide is 1:0.5 to 2:10 to 50.
Alternatively, the molar ratio of AgY, MZ and hydrogen halide is 1:0.5 to 2:12 to 45.
Alternatively, the molar ratio of AgY, MZ and hydrogen halide is 1:1:12 to 45.
Alternatively, the molar ratio of AgY and hydrogen halide is independently selected from any of 1.
In the present application, the hydrogen halide must be first prepared with AgY and MZ for use in solution L2. The hydrogen halide plays a role in promoting complete ionization of Ag and preventing the presence of AgY impurities; in addition, the addition of the hydrogen halide can reduce halogen ion vacancy, so that the surface defects of the nanocrystal are reduced, the optical performance of the nanocrystal is improved, and the quantum yield is improved.
Optionally, in step (S100), the concentration of CsX is 0.1mmol/mL to 0.5mmol/mL.
Optionally, in step (S100), the concentration of CsX is 0.1mmol/mL to 0.2mmol/mL.
Optionally, in step (S100), the concentration of CsX is 0.17mmol/mL.
Wherein, the concentration of CsX is calculated by the number of moles of Cs element contained therein.
Alternatively, in step (S200), the concentration of AgY is 0.01mmol/mL to 0.02mmol/mL.
Alternatively, in step (S200), the AgY concentration is 0.014mmol/mL.
Alternatively, in the step (S300), in the mixed solution of the solution L1 and the solution L2, the molar ratio of CsX to AgY is 0.5 to 1.5:1.
alternatively, the molar ratio of CsX to AgY is 0.8 to 1.2:1.
optionally, the molar ratio of CsX to AgY is 0.8 to 1:1.
wherein, the mole number of CsX is calculated as the mole number of Cs element contained therein.
Optionally, in the step (S300), the reaction temperature is 140 to 200 ℃ and the reaction time is 5S to 30min.
Optionally, in the step (S300), the reaction temperature is 150 to 170 ℃ and the reaction time is 5S to 10min.
Alternatively, in the step (S300), the temperature of the reaction is 160 ℃, and the time of the reaction is 10S.
Optionally, the temperature of the reaction is independently selected from any value of 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, 190 ℃, 200 ℃ or a range value between any two.
Optionally, the time of the reaction is independently selected from any of 5s, 8s, 10s, 1min, 2min, 5min, 7min, 10min, 12min, 15min, 17min, 20min, 22min, 25min, 27min, 30min, or a range between any two.
Optionally, the step (S100) comprises: heating a mixture containing a precursor CsX and an organic solvent to obtain a solution L1;
the organic solvent is at least one of octadecene and dimethyl sulfoxide;
the heating temperature is 50-200 ℃.
Optionally, the temperature of the heating is 120 ℃.
Alternatively, a mixture containing the precursor CsX and the organic solvent is heated, stirred, and dissolved to obtain a solution L1.
Optionally, mixing Cs 2 CO 3 One or more of CsCl, csBr and CsI are combined and dissolved in a flask by octadecene through heating and stirring to obtain a precursor solution.
Optionally, the step (S200) comprises: heating a mixture containing AgY, MZ, hydrogen halide, organic solvent and organic ligand to obtain a solution L2;
the organic solvent is at least one of octadecene and dimethyl sulfoxide;
the organic ligand is selected from at least one of oleic acid and oleylamine;
the heating temperature is 100-300 ℃.
Optionally, the temperature of the heating is 160 ℃.
Alternatively, a mixture containing AgY, MZ, hydrogen halide, an organic solvent and an organic ligand is heated and stirred under an inert gas atmosphere to dissolve, thereby obtaining a solution L2.
Optionally, the inert gas is selected from at least one of nitrogen, helium, and argon.
Alternatively, the amount of hydrogen halide used is 1mmol to 100mmol.
Alternatively, the amount of hydrogen halide used is 4mmol to 15mmol.
Alternatively, in step (S300), the addition is injection of the solution L1 into the solution L2.
Alternatively, in step (S300), the cooling is cooling with an ice-water mixture.
Optionally, in the step (S300), after cooling, centrifuging to obtain the lead-free halide double perovskite nanocrystal.
Optionally, the rotation speed of the centrifugation is 5000-12000 rmp.
Optionally, the rotation speed of the centrifugation is 10000rmp.
According to a second aspect of the present application, there is provided a lead halide-free double perovskite nanocrystal. The lead-free halide double perovskite nanocrystalline is synthesized by a precursor and halide through a thermal injection method, and the synthesized nanocrystalline is dispersed in an organic solvent, closely arranged under TEM observation and uniformly dispersed; the LED chip is excited to emit light with two different colors; the luminous mechanism is changed, the luminous efficiency is greatly improved, and the quantum yield is greatly improved.
The lead-free halide double perovskite nano crystal prepared by the preparation method is provided.
Optionally, the lead-free halide double perovskite nanocrystal has a chemical formula of Cs 2 AgMX’ 6 。
Wherein M is selected from Bi and/or In;
x' is a halide anion.
Optionally, the lead-free halide double perovskite nanocrystal has a chemical formula of Cs 2 AgBiBr 6 。
Optionally, the quantum yield of the lead-free halide double perovskite nanocrystal is 0.7% to 12%.
Optionally, the quantum yield of the lead-free halide double perovskite nanocrystal is 0.75% to 12%.
Optionally, the quantum yield of the lead-free halide double perovskite nanocrystal is 0.8% to 12%.
Optionally, the size of the lead-free halide double perovskite nanocrystal is 9 nm-20 nm.
Optionally, the size of the lead-free halide double perovskite nanocrystal is 9 nm-16 nm.
The beneficial effects that this application can produce include:
according to the preparation method of the lead-free halide double perovskite nanocrystalline, the proportion of hydrogen halide is adjusted, so that the emission spectrum is adjusted, the light-emitting color under the irradiation of a blue light chip is changed from red to green, the photoluminescence quantum yield (PLQY) is obviously improved, and compared with the maximum value reported in the literature, the maximum value is improved by one order of magnitude, and the maximum value is the highest value of the pure phase of the existing known perovskite nanocrystalline. The concentration of the hydrogen halide can change the luminescence mechanism of the double perovskite nanocrystalline, thereby greatly improving the luminescence efficiency and the quantum yield, simultaneously regulating and controlling the spectrum, realizing the conversion of the luminescence color, and effectively solving the problem of low quantum yield of the lead-free double perovskite nanocrystalline. The perovskite nanocrystalline material obtained by the preparation method through component adjustment is uniform in components and size, remarkably improves the luminous efficiency, realizes spectrum adjustment and conversion of luminous color, is environment-friendly, harmless to human bodies, good in stability in moisture and oxygen and has good application prospect.
Drawings
FIG. 1 is a schematic structural diagram of a lead-free halide double perovskite nanocrystal;
FIG. 2 is a TEM image (100 nm) of a nanocrystal sample # 1 prepared by adding 4.6mmol of hydrogen halide;
FIG. 3 is a TEM image (100 nm) of nanocrystalline sample # 2 prepared by adding 9.1mmol of hydrogen halide;
FIG. 4 is a TEM image (100 nm) of a nanocrystalline sample # 3 prepared by adding 11.4mmol of hydrogen halide;
FIG. 5 is a TEM image (100 nm) of a nanocrystal sample # 4 prepared by adding 13.7mmol of hydrogen halide;
fig. 6 is a graph showing a change in quantum yield.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The materials in the examples of this application were purchased commercially unless otherwise specified, and the test methods were performed by conventional methods and the equipment set up was as recommended by the manufacturer.
The analysis method in the examples of the present application is as follows:
the Transmission Electron Microscope (TEM) analysis adopts a JEM2100, and the representation of the microscopic morphology is carried out under the analysis condition of 300KV voltage.
The quantum yield was measured in a PLQYs test system (QE-2100) using an integrating sphere.
Quantum yield = (number of molecules of product produced)/(number of quantum absorbed).
Cs 2 AgMX’ 6 The schematic diagram of the crystal structure of (1) is shown in figure, a halogen atom X' is used as a vertex angle to construct a regular octahedron, ag and M respectively occupy the center of the octahedron alternately, and Cs occupies the face center position.
Example 1
(1) 2mmol of Cs 2 CO 3 Mixing, heating, stirring and dissolving 20mL of octadecene and 3mL of oleic acid in a flask at the heating temperature of 120 ℃ to obtain a precursor solution L1;
(2) 0.367mmol of AgBr and 0.367mmol of BiBr 3 Heating 20mL of octadecene, 3mL of organic ligand oleylamine and 3mL of organic ligand oleic acid under the atmosphere of argon gas, stirring and dissolving in a flask, heating to 160 ℃, and adding 4.6mmol of HBr to obtain a halide solution L2;
(3) 2mLCs 2 CO 3 The precursor solution L1 is injected into the solution L2, wherein Cs 2 CO 3 And AgBr in a molar ratio of 0.47, at 160 ℃ for 10s;
(4) Cooling the reacted solution in ice water, cooling the solution to room temperature, centrifuging with centrifuge at rotation speed of 10000rmp to obtain nanocrystalline precipitate with chemical formula of Cs 2 AgBiBr 6 And recorded as sample # 1. FIG. 2 is a TEM image (100 nm) of sample No. 1, and it can be seen that the nanocrystals were uniformly dispersed and uniform in size, with a size of about 9.74nm. The mechanism of luminescence is the same as that reported (see Dey A, richter A F, debnath T, et al. Transfer of Direct to induced Bound inductances by Electron interference Scattering in Cs2AgBiBr6 Double Perovskentin and ions [ J]ACS nano,2020,14 (5): 5855-5861.) with quantum yield of 0.7% and red light emission under the excitation of a blue light chip.
Example 2
(1) Mixing 2 mmoles of Cs 2 CO 3 Mixing 20mL of octadecene and 3mL of oleic acid, heating, stirring and dissolving in a flask at the heating temperature of 120 ℃ to obtain a precursor solution L1;
(2) 0.367mmol of AgBr and 0.367mmol of BiBr 3 Heating 20mL of octadecene, 3mL of organic ligand oleylamine and 3mL of organic ligand oleic acid under the atmosphere of argon gas, stirring and dissolving in a flask, heating to 160 ℃, and adding 9.1mmol of HBr to obtain a halide solution L2;
(3) 2mLCs 2 CO 3 Injecting the precursor solution L1 into the solution L2, wherein Cs 2 CO 3 And AgBr in a molar ratio of 0.47, at 160 ℃ for 10s;
(4) Putting the reacted solution into ice water for cooling, cooling the solution to room temperature, centrifuging by using a centrifuge,centrifuging at 10000rmp to obtain nanocrystalline precipitate with chemical formula of Cs 2 AgBiBr 6 And is recorded as sample # 2. FIG. 3 is a TEM image (100 nm) of sample 2# and it can be seen that the nanocrystals were uniformly dispersed and uniform in size, with a size of about 9.75nm. The light-emitting mechanism of the luminescent material begins to change, the radiation luminescence of a trap state caused by defects is converted into the radiation luminescence of a non-trap state, the quantum yield is 6.8%, and green light is emitted under the excitation of a blue light chip.
Example 3
(1) Mixing 2 mmoles of Cs 2 CO 3 Mixing 20mL of octadecene and 3mL of oleic acid, heating, stirring and dissolving in a flask at the heating temperature of 120 ℃ to obtain a precursor solution L1;
(2) 0.367mmol of AgBr and 0.367mmol of BiBr 3 Heating, stirring and dissolving 20mL of octadecene, 3mL of organic ligand oleylamine and 3mL of organic ligand oleic acid in a flask under the atmosphere of argon gas, heating to 160 ℃, and adding 11.4mmol of HBr to obtain a halide solution L2;
(3) 2mLCs 2 CO 3 The precursor solution L1 is injected into the solution L2, wherein Cs 2 CO 3 And AgBr in a molar ratio of 0.47, at 160 ℃ for 10s;
(4) Cooling the reacted solution in ice water, cooling the solution to room temperature, centrifuging with centrifuge at rotation speed of 10000rmp to obtain nanocrystalline precipitate with chemical formula of Cs 2 AgBiBr 6 And is recorded as sample # 3. Fig. 4 is a TEM image (100 nm) of sample 3# and it can be seen that the nanocrystals were uniformly dispersed and of uniform size, with a size of about 9.90nm and a quantum yield of 9.0%, and emitted green light under excitation of a blue chip.
Example 4
(1) Mixing 2 mmoles of Cs 2 CO 3 Mixing 20mL of octadecene and 3mL of oleic acid, heating, stirring and dissolving in a flask at the heating temperature of 120 ℃ to obtain a precursor solution L1;
(2) 0.367mmol of AgBr and 0.367mmol of BiBr 3 20mL of octadecene, 3mL of organic ligand oleylamine and 3mL of organic ligand oleic acid are heated, stirred and dissolved in a flask under the atmosphere of argon gas, and the heating temperature is 16 DEGAdding 13.7mmol HBr at 0 ℃ to obtain a halide solution L2;
(3) 2mLCs 2 CO 3 The precursor solution L1 is injected into the solution L2, wherein Cs 2 CO 3 And AgBr in a molar ratio of 0.47, at 160 ℃ for 10s;
(4) Cooling the reacted solution in ice water, cooling the solution to room temperature, centrifuging with centrifuge at rotation speed of 10000rmp to obtain nanocrystalline precipitate with chemical formula of Cs 2 AgBiBr 6 And is recorded as sample # 4. Fig. 5 is a TEM image (100 nm) of sample 3# and it can be seen that the nanocrystals were uniformly dispersed and uniform in size, with a size of about 15.92nm and a quantum yield of 11.6%, and emitted green light under excitation of a blue chip.
Fig. 6 is a graph showing the quantum yield variation of the nanocrystals of samples # 1 to # 4 according to the amount of hydrogen halide, from which it can be seen that the quantum yield is significantly improved according to the increase of the amount of hydrogen halide.
Comparative example 1
Cs prepared by supersaturated recrystallization methods reported to date 2 AgBiBr 6 Nanocrystals, such as those described in Yang B, chen J, yang S, et al, lead-free silver-bismuth halide double perovskitans chrystals [ J]Angewandte Chemie,2018,130 (19): 5457-5461, with a quantum yield of only 0.7%.
Comparative example 2
((1) mixing 2mmol of Cs 2 CO 3 Mixing, heating, stirring and dissolving 20mL of octadecene and 3mL of oleic acid in a flask at the heating temperature of 120 ℃ to obtain a precursor solution L1;
(2) 0.367mmol of AgBr and 0.367mmol of BiBr 3 Heating, stirring and dissolving 20mL of octadecene, 3mL of organic ligand oleylamine and 3mL of organic ligand oleic acid in a flask under the atmosphere of argon gas, wherein the heating temperature is 160 ℃, and no halide is added to obtain a solution L2;
(3) 2mLCs 2 CO 3 The precursor solution L1 is injected into the solution L2, wherein Cs 2 CO 3 And AgBr in a molar ratio of 0.47, at 160 ℃ for 10s;
(4) Dissolving after reactionCooling the solution in ice water, cooling to room temperature, centrifuging at 10000rmp to obtain nanocrystalline precipitate with chemical formula of Cs 2 AgBiBr 6 The quantum yield was 0%.
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of lead-free halide double perovskite nanocrystalline is characterized by comprising the following steps;
(S100) obtaining a solution L1 of a precursor CsX;
(S200) obtaining a solution L2 containing AgY, MZ and hydrogen halide;
(S300) adding the solution L1 into the solution L2, mixing, reacting, and cooling to obtain the lead-free halide double perovskite nano crystal;
wherein X is selected from CO 3 2- At least one of halogen anion;
m is selected from Bi and/or In;
y and Z are independently selected from at least one of halide anions.
2. The production method according to claim 1, wherein, in the step (S200),
the molar ratio of AgY, MZ and hydrogen halide is 1:0.5 to 2:10 to 50;
preferably, the molar ratio of AgY, MZ and hydrogen halide is 1:0.9 to 1.1:12 to 45.
3. The method according to claim 1, wherein in the step (S100), the concentration of CsX is 0.1mmol/mL to 0.5mmol/mL;
in the step (S200), the AgY concentration is 0.01 mmol/mL-0.02 mmol/mL.
4. The method according to claim 1, wherein in the step (S300), in the mixed solution of the solution L1 and the solution L2, the molar ratio of CsX to AgY is 0.5 to 1.5:1;
preferably, the molar ratio of CsX to AgY is 0.8 to 1.2:1.
5. the method of claim 1, wherein the reaction temperature is 140 ℃ to 200 ℃ and the reaction time is 5S to 30min in the step (S300).
6. The method of claim 1, wherein the step (S100) includes: heating a mixture containing a precursor CsX and an organic solvent to obtain a solution L1;
the organic solvent is at least one of octadecene and dimethyl sulfoxide;
the heating temperature is 50-200 ℃.
7. The method of claim 1, wherein the step (S200) includes: heating a mixture containing AgY, MZ, hydrogen halide, organic solvent and organic ligand to obtain a solution L2;
the organic solvent is at least one of octadecene and dimethyl sulfoxide;
the organic ligand is selected from at least one of oleic acid and oleylamine;
the heating temperature is 100-300 ℃.
8. The lead-free halide double perovskite nanocrystal prepared by the preparation method according to any one of claims 1 to 7.
9. The lead-free halide double perovskite nanocrystal of claim 8, wherein the quantum yield of the lead-free halide double perovskite nanocrystal is from 0.7% to 12%.
10. The lead-free halide double perovskite nanocrystal of claim 8, wherein the lead-free halide double perovskite nanocrystal is from 9nm to 20nm in size.
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