CN112798545B - Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof - Google Patents

Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof Download PDF

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CN112798545B
CN112798545B CN201911105809.XA CN201911105809A CN112798545B CN 112798545 B CN112798545 B CN 112798545B CN 201911105809 A CN201911105809 A CN 201911105809A CN 112798545 B CN112798545 B CN 112798545B
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李�灿
石明
李仁贵
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention discloses an inorganic perovskite material with continuously adjustable absorption spectrum, and preparation and application thereof, wherein the perovskite material comprises: 1) one or more monovalent metal cations [ A]+(ii) a 2) One or more trivalent metal cations [ B]3+(ii) a 3) One or more trivalent metal cations [ B']3+(ii) a 4) One or more halogen anions [ X ]]‑. Having a chemical formula of [ A]x[B]y[B']z[X]nWherein y + z is 2x/3, n is 3x, x>0. The material can realize continuous adjustment of absorption spectrum through modulation of different ion components, and the preparation method is simple, convenient and environment-friendly. The perovskite material is expected to be applied to the fields of photocatalysis, photoelectric detection, solar cells, laser, light emitting diodes and the like.

Description

Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof
Technical Field
The invention belongs to the field of perovskite materials, and particularly relates to an inorganic perovskite material with a continuously adjustable absorption spectrum, as well as preparation and application thereof.
Background
For recent years, lead methylamine halides (MAPbX)3) The representative halide perovskite materials have attracted considerable attention in various fields such as solar cells and light-emitting devices due to their excellent photoelectric properties (chem.soc.rev.,2016,45, 655-689; Acc.chem.Res.2016,49, 528-535). The material has the unique properties of adjustable band gap structure, high light absorption coefficient, high carrier mobility, long carrier diffusion length and the like, so that the material has wide application prospect in the fields of solar cells, light-emitting diodes, photoelectric detection, laser, photocatalysis and the like. However, the toxicity of lead and the problems of environmental pollution, the photostability of organic groups such as methylamino groups, etc. have greatly limited the applications of such materials. Therefore, the development of novel inorganic non-lead perovskite materials is an important approach for the future development of perovskite materials to industrial application.
In recent years, some studies have reported that lead is replaced by an element having properties similar to those of lead in the periodic table, and that methylamino and the like are replaced by an inorganic metal ion such as Sn2+、Bi3+Substitute for Pb2+Synthetic MASnX3(X＝Cl,Br,I)、MA3Bi2X9(X ═ Cl, Br, I), although reducing the toxicity of such materials, the stability and optical properties of the materials are still not ideal (j. mater. chem.a,2017,5, 11436-; some studies have reported that inorganic Cs ions replace the methyl amino group of CsPbX3Perovskite materials such as (X ═ Cl, Br, I) have improved stability to some extent, but their photoelectric properties are greatly reduced (j.am.chem.soc.2016,138, 15829-15832). Therefore, the development of a novel non-lead inorganic perovskite material which is non-toxic, stable and has wide spectral absorption has important significance in a plurality of fields such as solar cells, light-emitting devices and the like.
Disclosure of Invention
The invention aims to provide an inorganic perovskite material which is low in toxicity, stable and continuously adjustable in absorption spectrum, aiming at the problems of high toxicity, poor stability and narrow spectral absorption range of the conventional halide perovskite semiconductor material. The chemical formula of the material is [ A ]]x[B]y[B']z[X]nComprising one or more monovalent cations [ A]+One or more trivalent cations [ B ]]3+And one or more trivalent cations [ B']3+One or more halogen anions [ X ]]-Wherein y + z is 2x/3, n is 3x, x>0。
Specifically, the inorganic perovskite material avoids commonly adopted lead ions by adopting one or more trivalent cations, so that the toxicity of the material is reduced; inorganic metal ions are adopted, and organic groups such as methylamine and the like are avoidedTherefore, the stability of the material is improved. At the same time, compared with the composition containing single trivalent [ B ]]3+Or [ B']3+Ions by modulating metal cations [ B]3+And [ B']3+The absorption spectrum can be continuously adjusted in the visible light range.
Thus, the present invention provides a class of inorganic perovskite materials [ A ]]x[B]y[B']z[X]nThe material comprises:
1) one or more monovalent metal cations [ A]+；
2) One or more first trivalent metal cations [ B]3+；
3) One or more secondary trivalent metal cations [ B']3+；
4) One or more halogen anions [ X ]]-。
The invention also provides a method for preparing the inorganic perovskite material, which comprises the following steps:
1) reacting a halide metal salt AX, BX3，B'X3Dissolving into acid solution according to different molar ratios, and stirring for a certain time within a given temperature range.
2) And (3) after the reaction system in the step (1) is subjected to constant temperature reaction at a specific reaction temperature for a certain time, stopping heating and stirring, and cooling to a certain temperature.
3) And centrifuging the cooled product, removing the supernatant, and drying to obtain the reaction product.
Further, the halide metal salt AX, BX in step 13，B'X3In a molar ratio of x: y: z, wherein y + z is 2x/3, x>0。
Further, the acid in the step 1 includes one or more of hydrochloric acid, sulfuric acid, nitric acid, acetic acid, hydrobromic acid, hydroiodic acid, and the like, and the concentration range of the acid is 0.5-15 mol/L.
Further, the stirring temperature in the step 1 is 0-200 ℃ (preferably 25-160 ℃), and the stirring time is 1-300 minutes (preferably 30-120 minutes).
Further, the specific reaction temperature range in the step 2 is 0-300 ℃ (preferably 25-160 ℃); the reaction time is 1-600 minutes (preferably 30-120 minutes); the temperature range of the cooled liquid is 0-300 ℃ (preferably 25-80 ℃).
Further, the drying method in step 3 is one or more of vacuum drying, gas protection drying, freeze drying and the like. The gas used for gas protection drying is one or more mixed gas of nitrogen, argon, hydrogen, oxygen, carbon dioxide and the like.
Furthermore, in the step 3, the drying temperature is 10-100 ℃ (preferably 60-80 ℃), and the drying time is 0.1-24 hours (preferably 12-24 hours).
The novel inorganic perovskite material can be used in the fields of photocatalysis, photoelectric detection, solar cells, laser, light emitting diodes and the like.
The invention has the following beneficial effects:
1) the invention provides a novel inorganic perovskite material [ A]x[B]y[B']z[X]nThe method has the advantages of low toxicity, stability, continuous and adjustable absorption spectrum in a visible light range and the like, and the preparation method is simple, convenient and environment-friendly.
2) The novel inorganic perovskite material provided by the invention is expected to be applied to the fields of photocatalysis, photoelectric detection, solar cells, laser, light emitting diodes and the like.
Drawings
FIG. 1 shows Cs according to an embodiment of the present invention3SbxBi1-xBr9XRD pattern of (a);
FIG. 2 shows Cs according to an embodiment of the present invention3SbxBi1-xBr9An XRD pattern of 2 theta at 20-35 degrees;
FIG. 3 shows Cs according to an embodiment of the present invention3SbxBi1-xBr9Ultraviolet-visible diffuse reflectance pattern of (a).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following will further illustrate the contents of the present invention with reference to the examples.
The invention relates to a first-class suckerInorganic perovskite material [ A ] with continuously adjustable spectral absorption]x[B]y[B']z[X]nThe preparation method comprises the following steps: reacting halide metal salt AX (such as CsBr), BX3(e.g., SbBr)3)、B'X3(e.g., BiBr)3) Dissolving the mixture into an acid solution according to different molar ratios, and stirring the mixture for a certain time within a given temperature range; reacting the reaction system at a constant temperature for a certain time at a specific reaction temperature, stopping heating and stirring, and cooling to a certain temperature; and centrifuging the cooled product, removing the supernatant, and drying to obtain the reaction product.
Example 1
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:0.25:1.75, the chemical formula of the inorganic perovskite material is Cs3Sb0.25Bi1.75Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:0.25:1.75) was added to a round-bottomed flask containing hydrobromic acid, and stirred at room temperature for 30 min.
2) The reaction system is stirred to completely dissolve reactants, the temperature is kept at 150 ℃ for reaction for 2h, heating and stirring are stopped, and the reaction system is naturally cooled to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, performing centrifugal separation, pouring out supernatant, and drying the precipitate at 80 ℃ for 12h to obtain a reaction product Cs3Sb0.25Bi1.75Br9。
Example 2
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:0.5:1.5, the chemical formula of the inorganic perovskite material is Cs3Sb0.5Bi1.5Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:0.5:1.5) was added to a round-bottomed flask containing hydrobromic acid, and the mixture was stirred at room temperatureStirring for 30 min.
2) The reaction system is stirred to completely dissolve reactants, the temperature is kept at 150 ℃ for reaction for 2h, heating and stirring are stopped, and the reaction system is naturally cooled to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, performing centrifugal separation, pouring out supernatant, and drying the precipitate at 80 ℃ for 12h to obtain a reaction product Cs3Sb0.5Bi1.5Br9。
Example 3
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:0.75:1.25, the chemical formula of the inorganic perovskite material is Cs3Sb0.75Bi1.25Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:0.75:1.25) was added to a round-bottomed flask containing hydrobromic acid, and stirred at room temperature for 30 min.
2) The reaction system is stirred to completely dissolve reactants, the temperature is kept at 150 ℃ for reaction for 2h, heating and stirring are stopped, and the reaction system is naturally cooled to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, performing centrifugal separation, pouring out supernatant, and drying the precipitate at 80 ℃ for 12h to obtain a reaction product Cs3Sb0.75Bi1.25Br9。
Example 4
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:1:1, the chemical formula of the inorganic perovskite material is Cs3SbBiBr9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:1:1) was added to a round-bottom flask charged with hydrobromic acid and stirred at room temperature for 30 min.
2) Heating the reaction system to 150 ℃ while stirring, dissolving all reactants, keeping the temperature for reaction for 2 hours, stopping heating and stirring, and naturally cooling to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, performing centrifugal separation, pouring out supernatant, and drying the precipitate at 80 ℃ for 12h to obtain a reaction product Cs3SbBiBr9。
Example 5
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:1.25:0.75, the chemical formula of the inorganic perovskite material is Cs3Sb1.25Bi0.75Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:1.25:0.75) was added to a round-bottomed flask containing hydrobromic acid, and stirred at room temperature for 30 min.
2) Heating the reaction system to 150 ℃ while stirring, dissolving all reactants, keeping the temperature for reaction for 2 hours, stopping heating and stirring, and naturally cooling to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, centrifuging at 5000rpm for 1min, pouring out the supernatant, and drying the precipitate in an oven at 80 ℃ for 12h to obtain a reaction product Cs3Sb1.25Bi0.75Br9。
Example 6
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:1.5:0.5, the chemical formula of the inorganic perovskite material is Cs3Sb1.5Bi0.5Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:1.5:0.5) was charged into a 100mL round-bottom flask containing 20mL hydrobromic acid, and stirred at room temperature for 30 min.
2) Heating the reaction system to 150 ℃ while stirring, dissolving all reactants, keeping the temperature for reaction for 2 hours, stopping heating and stirring, and naturally cooling to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, centrifuging at 5000rpm for 1min, pouring out the supernatant, and drying the precipitate in an oven at 80 ℃ for 12h to obtain a reaction product Cs3Sb1.5Bi0.5Br9。
Example 7
When [ A ] is]+Is Cs+、[B]3+Is Sb3+、[B']3+Is Bi3+When the molar ratio of x, y and z is 3:1.75:0.25, the chemical formula of the inorganic perovskite material is Cs3Sb1.75Bi0.25Br9The synthesis steps are as follows:
1) weighing a certain amount of CsBr and SbBr3And BiBi3(molar ratio 3:1.75:0.25) was added to a round-bottomed flask containing hydrobromic acid, and stirred at room temperature for 30 min.
2) Heating the reaction system to 150 ℃ while stirring, dissolving all reactants, keeping the temperature for reaction for 2 hours, stopping heating and stirring, and naturally cooling to room temperature.
3) Pouring the cooled reaction solution and the cooled product into a centrifuge tube, centrifuging at 5000rpm for 1min, pouring out the supernatant, and drying the precipitate in an oven at 80 ℃ for 12h to obtain a reaction product Cs3Sb1.75Bi0.25Br9。
The foregoing is illustrative of the present invention and is not to be construed as limiting thereof, and all such modifications, equivalents and improvements that are within the spirit of the invention are intended to be included therein.

Claims (5)

1. An inorganic perovskite material with continuously adjustable absorption spectrum, which is characterized in that the chemical formula of the perovskite material is Cs3SbyBi2-yBr9Y is more than or equal to 0.25 and less than or equal to 1.75, and the absorption spectrum of the perovskite material can be continuously adjusted by adjusting the value of y;
the preparation method of the perovskite material comprises the following steps:
1) the halide metal salts CsBr and SbBr3And BiBr3Dissolving the mixture into an acid solution according to a molar ratio of 3: y (2-y), and stirring for 1-300 minutes at the temperature of 0-200 ℃; wherein y is more than or equal to 0.25 and less than or equal to 1.75;
2) after the reaction system in the step 1) is reacted at the constant temperature of 150 ℃ for a certain time, stopping heating and stirring, and cooling to a certain temperature;
3) and centrifuging the cooled product, removing the supernatant, and drying to obtain the reaction product.
2. The perovskite material of claim 1, wherein the acid in step 1) is one or more of hydrobromic acid, sulfuric acid and nitric acid, and the concentration of the acid is in the range of 0.5-15 mol/L;
in the step 1), the stirring temperature is 25-160 ℃, and the stirring time is 30-120 minutes;
the reaction time in the step 2) is 1-600 minutes; the temperature range of the cooled liquid is 25-80 ℃.
3. The perovskite material of claim 1, wherein the drying method in step 3) is vacuum drying or gas-shielded drying; the gas used for gas protection drying is one or more of nitrogen, argon and carbon dioxide;
in the step 3), the drying temperature is 10-100 ℃, and the drying time is 0.1-24 hours.
4. The perovskite material of claim 3,
the reaction time in the step 2) is 30-120 minutes;
in the step 3), the drying temperature is 60-80 ℃, and the drying time is 12-24 hours.
5. Use of an inorganic perovskite material as defined in any one of claims 1 to 4 for photocatalysis, photodetection elements, solar cells, laser elements or light emitting diodes.
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