CN115044369B - Ordered vacancy leadless double perovskite micro-crystal fluorescent material and preparation method thereof - Google Patents
Ordered vacancy leadless double perovskite micro-crystal fluorescent material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an ordered vacancy leadless double perovskite micro-crystal fluorescent material and a preparation method thereof, belonging to the technical field of leadless perovskite fluorescent materials. The chemical formula of the microcrystalline fluorescent material is Rb 2 ZrCl 6‑x Br x ，0X is more than or equal to 2, the excitation wavelength is in the range of 200 nm-300 nm, the emission wavelength is in the range of 440 nm-500 nm, and the fluorescence quantum yield is in the range of 60% -95%; with RbBr powder, rbCl powder and ZrCl 4 And adding acetone into the powder serving as a raw material for grinding to obtain the micro-crystal fluorescent material. The microcrystalline fluorescent material has the characteristics of no toxicity, tunable luminous band gap, high fluorescence quantum yield, wide spectrum emission, low cost, stable optical characteristics and the like, and the preparation method is simple to operate, short in reaction time, suitable for mass production and has a huge application prospect.
Description
Technical Field
The invention relates to an ordered vacancy leadless double perovskite micro-crystal fluorescent material and a preparation method thereof, belonging to the technical field of leadless perovskite fluorescent materials.
Background
Lead halide perovskite ABX 3 (A＝Rb、Cs、CH 3 NH 2 (MA)、CH 4 N 2 (FA); b=pb; x=cl, br, I) has a wide application prospect in the fields of solar cells, light emitting diodes, photoelectric detection, laser, photocatalysis, X-ray imaging, and the like due to its excellent photoelectric characteristics. However, the toxicity of lead elements restricts the application process. Thus, new green lead-free perovskite materials are explored through non-toxic element replacement strategies. For example, using ns with equivalent value 2 np 0 Sn of external electronic structure 2+ And Ge (Ge) 2+ Element replacement strategy and use of Bi of different valence states 3+ And Sb (Sb) 3+ Element replacement policy. However, the optical properties and stability of these materials are often not as good as expected, severely limiting further applications. Therefore, it is a challenge to solve the problem of lead toxicity while ensuring excellent photoelectric properties of the material.
Recently reported green leadless double perovskites, such as Cs 2 AgBiX 6 、Cs 2 AgInX 6 Cs 2 AgSbX 6 (x=cl, br, I), belonging to the three-dimensional perovskite structure, they are indirect band gaps, while luminescence belongs to forbidden transitions, which results in their inefficient quantum yield, greatly limiting green commercial illumination. Ordered vacancy double perovskite, a new kind of calciumThe titanium ore architecture, in which two divalent atoms are replaced by a single tetravalent atom, has an ordered vacancy double perovskite forming 50% of B-site atom vacancies relative to a conventional three-dimensional perovskite structure. The ordered vacancy double perovskite has a unique zero-dimensional electronic structure and has stronger space trapping capacity in theory, so that the effective radiation transition of excitons is greatly increased, and high-efficiency fluorescence emission can be generated. However, vacancy ordered double perovskites, such as Cs, are currently reported 2 SnI 6 、K 2 TeBr 6 Rb 2 SnI 6 The quantum yield is generally low, so that the novel ordered vacancy double perovskite is developed to be close to theoretical fluorescence high-efficiency emission, and the ideal commercial green illumination requirement is achieved, and the novel ordered vacancy double perovskite is a scientific problem to be solved urgently at present.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an ordered vacancy leadless double perovskite micro-crystal and a preparation method thereof, and the micro-crystal fluorescent material is Rb 2 ZrCl 6-x Br x (x is more than or equal to 0 and less than or equal to 2), has the characteristics of no toxicity, tunable luminous band gap, high fluorescence quantum yield, wide spectrum emission, low cost, stable optical characteristics and the like, and has great application prospect; the preparation method of the micron-sized crystal fluorescent material by adopting a wet grinding solid phase reaction method has the advantages of simple operation and short reaction time, and is suitable for batch production.
The aim of the invention is achieved by the following technical scheme.
Ordered vacancy leadless double perovskite micro-crystalline fluorescent material, wherein chemical formula of micro-crystalline fluorescent material is Rb 2 ZrCl 6-x Br x X is more than or equal to 0 and less than or equal to 2, the excitation wavelength is in the range of 200 nm-300 nm, the emission wavelength is in the range of 440 nm-500 nm, and the fluorescence quantum yield is in the range of 60% -95%.
Further, rb 2 ZrCl 6-x Br x In x=0.8 to 1.5, the fluorescence quantum yield reaches 85% or more.
Further, the particle size of the microcrystalline fluorescent material is 0.05-0.35 μm.
The preparation method of the microcrystalline fluorescent material comprises the following specific steps:
the RbBr powder, the RbCl powder and the ZrCl are mixed according to the stoichiometric ratio 4 Adding the powder into a mortar, adding acetone, and then carrying out wet grinding in one direction, wherein the acetone is added intermittently in the grinding process because of volatility, and removing the acetone after grinding for not less than 5min to obtain the micro-crystal fluorescent material.
Further, according to ZrCl 4 The powder and acetone are 1mol: (2 mL to 5 mL) acetone was added to the mill.
Further, the grinding speed is 25 r/min-40 r/min, acetone is added into the mortar after the acetone volatilizes for 2 min-5 min each time, and the acetone is repeatedly added for 2-4 times.
The beneficial effects are that:
(1) The invention relates to a micron crystal fluorescent material Rb 2 ZrCl 6-x Br x The space group is Fm-3m, and the space group is separated into a co-angular octahedron [ ZrCl ] by rubidium atoms 6-x Br x ] 2- Thus, a zero-dimensional structure is formed, a strong trapping effect is generated on excitons, and the self-trapping luminescence is characterized by wide-spectrum emission and large Stokes shift, and has high fluorescence quantum yield. In the present application, the microcrystalline fluorescent material Rb consists of Rb, zr, cl and Br 2 ZrCl 6-x Br x The excitation wavelength is within the range of 200 nm-300 nm, the emission wavelength is within the range of 440 nm-500 nm, and the fluorescence quantum yield is within the range of 60% -95%.
(2) As is known from the first principle calculation, the optical band gap is generated in the public angle octahedron [ ZrCl ] 6-x Br x ] 2- In the method, 3p orbitals of chlorine atoms and bromine atoms provide valence band construction, and as the energy of the 3p orbitals of the chlorine atoms is higher, when the replacement content of bromine elements is increased, the valence band becomes low, the corresponding optical band gap is reduced, and a red shift is generated, so that an inherent band gap luminescence mechanism provides theoretical support for realizing band gap regulation.
(3) According to the atomic force microscopy study of the solid state effect of the Gerd Kaupp group into the molecular level, the mechanosynthesis-based molecular solid state reaction can occur so easily from three requirements, including the long range anisotropic molecular migration allowed by the lattice, the product phase can be formed fast enough, and the crystal disintegrates to provide a fresh surface. The polishing method according to the present invention can provide the three aforementioned conditions, and thus can realize the production of a fluorescent material having good crystallinity. In addition, acetone is added in the grinding process, mainly because of the specific viscosity and high volatility of the acetone, the raw materials are more favorably in an atomic free state, and the crystallization nucleation process is easier to occur, so that the vacancy ordered perovskite with high crystallinity is obtained.
Drawings
FIG. 1 is an SEM image of an ordered vacancy leadless double perovskite micro crystal fluorescent material prepared in example 1.
FIG. 2 is a statistical plot of the particle size distribution of ordered vacancy leadless double perovskite micro-crystalline fluorescent material prepared in example 1.
FIG. 3 is a graph showing the comparison of the calculation of the band gap of the ultraviolet visible diffuse reflection spectrum of the ordered vacancy leadless double perovskite micro crystal fluorescent material prepared in examples 1 to 5.
FIG. 4 is an X-ray diffraction (XRD) contrast pattern of ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in examples 1-5.
Fig. 5 is a graph showing the comparison of fluorescence excitation spectra and emission spectra of ordered vacancy leadless double perovskite micro-crystalline fluorescent materials prepared in examples 1 to 5.
FIG. 6 is a graph of the fluorescence quantum yield spectrum of the ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in example 1.
FIG. 7 is a graph of the fluorescence quantum yield spectrum of the ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in example 2.
FIG. 8 is a graph of the fluorescence quantum yield spectrum of the ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in example 3.
FIG. 9 is a graph of the fluorescence quantum yield spectrum of the ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in example 4.
FIG. 10 is a graph of the fluorescence quantum yield spectrum of the ordered vacancy leadless double perovskite microcrystalline fluorescent material prepared in example 5.
Fig. 11 is a comparative graph of fluorescence emission spectra of the materials prepared in example 1, comparative example 1, and comparative example 2.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
Example 1
(1) 0.242g of RbCl powder and 0.233g of ZrCl powder are taken 4 Adding the powder into a mortar, and adopting a grinding rod to grind the powder clockwise for 3min at a grinding speed of 30r/min so as to fully mix the powder;
(2) Adding 5mL of acetone into a mortar, and then continuously grinding clockwise for 3min at a grinding speed of 40r/min to volatilize the acetone in the powder;
(3) Repeating the step (2) for three times, grinding for the last time until the acetone volatilizes, and drying for 2 hours at 80 ℃ to obtain the ordered vacancy leadless double perovskite micro-crystal fluorescent material, wherein the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 6 。
Rb 2 ZrCl 6 Is 259nm, and the emission peak is 445nm, with a large stokes shift, as shown in fig. 5.
As can be seen from the XRD patterns in FIG. 4, rb 2 ZrCl 6 The crystallinity is better, and the crystal structure is pure phase.
As can be seen from fig. 3, rb 2 ZrCl 6 Is 3.895eV.
From FIG. 6, rb can be seen 2 ZrCl 6 The fluorescence quantum yield of (2) reaches 81.2%.
As can be seen from fig. 1 and 2, rb 2 ZrCl 6 The particle size of the particles is normally distributed, and the particle size distribution range is 0.05 mu m to 0.35 mu m.
Example 2
(1) Taking 0.181g of RbCl powder, 0.083g of RbBr powder and 0.233g of ZrCl 4 Adding the powder into a mortar, and grinding clockwise for 3m at a grinding speed of 30r/min by adopting a grinding rodin, fully mixing the powder;
(2) Adding 5mL of acetone into a mortar, and then continuously grinding clockwise for 3min at a grinding speed of 30r/min to volatilize the acetone in the powder;
(3) Repeating the step (2) for three times, grinding for the last time until the acetone volatilizes, and drying for 2 hours at 80 ℃ to obtain the ordered vacancy leadless double perovskite micro-crystal fluorescent material, wherein the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 5.5 Br 0.5 。
Rb 2 ZrCl 5.5 Br 0.5 The excitation peak position of (2) is 276nm, the emission peak position is 464nm, and the excitation peak position has a larger Stokes shift, as shown in figure 5.
As can be seen from the XRD patterns in FIG. 4, rb 2 ZrCl 5.5 Br 0.5 The crystallinity is better, and the crystal structure is pure phase.
As can be seen from fig. 3, rb 2 ZrCl 5.5 Br 0.5 Is 3.866eV.
From FIG. 7, rb can be seen 2 ZrCl 5.5 Br 0.5 The fluorescence quantum yield of (3) reaches 73.3%.
From the particle size distribution statistics, rb 2 ZrCl 5.5 Br 0.5 The particle size of the particles is normally distributed, and the particle size distribution range is 0.03-0.37 mu m.
Example 3
(1) 0.121g of RbCl powder, 0.165g of RbBr powder and 0.233g of ZrCl powder are taken 4 Adding the powder into a mortar, and adopting a grinding rod to grind the powder clockwise for 3min at a grinding speed of 30r/min so as to fully mix the powder;
(2) Adding 5mL of acetone into a mortar, and then continuously grinding clockwise for 3min at a grinding speed of 30r/min to volatilize the acetone in the powder;
(3) Repeating the step (2) for three times, grinding for the last time until the acetone volatilizes, and drying for 2 hours at 80 ℃ to obtain the ordered vacancy leadless double perovskite micro-crystal fluorescent material, wherein the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 5 Br 1 。
Rb 2 ZrCl 5 Br 1 Is 277nm, and the emission peak is 469nm, with a large stokes shift, as shown in fig. 5.
As can be seen from the XRD patterns in FIG. 4, rb 2 ZrCl 5 Br 1 The crystallinity is better, and the crystal structure is pure phase.
As can be seen from fig. 3, rb 2 ZrCl 5 Br 1 The optical bandgap of (2) is 3.840eV.
From FIG. 8, rb can be seen 2 ZrCl 5 Br 1 The fluorescence quantum yield of (2) reaches 90.2%.
As can be seen from the particle size distribution statistics, b 2 ZrCl 5 Br 1 The particle size of the particles is normally distributed, and the particle size distribution range is 0.05 mu m to 0.36 mu m.
Example 4
(1) 0.060g of RbCl powder, 0.248g of RbBr powder and 0.233g of ZrCl powder are taken 4 Adding the powder into a mortar, and adopting a grinding rod to grind clockwise for 5min at a grinding speed of 30r/min to fully mix the powder;
(2) Adding 5mL of acetone into a mortar, and then continuously grinding clockwise for 4min at a grinding speed of 40r/min to volatilize the acetone in the powder;
(3) Repeating the step (2) for three times, grinding for the last time until the acetone volatilizes, and drying for 2 hours at 80 ℃ to obtain the ordered vacancy leadless double perovskite micro-crystal fluorescent material, wherein the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 4.5 Br 1.5 。
Rb 2 ZrCl 4.5 Br 1.5 The excitation peak position is 278nm, the emission peak position is 471nm, and the excitation peak position has larger Stokes shift, as shown in figure 5.
As can be seen from the XRD patterns in FIG. 4, rb 2 ZrCl 45 Br 15 The crystallinity is better, and the crystal structure is pure phase.
As can be seen from fig. 3, rb 2 ZrCl 4.5 Br 1.5 Is 3.810eV.
From FIG. 9, rb can be seen 2 ZrCl 4.5 Br 1.5 The fluorescence quantum yield of (2) reaches 89.0%.
From the particle size distribution statistics, rb 2 ZrCl 4.5 Br 1.5 The particle size of the particles is normally distributed, and the particle size distribution range is 0.03-0.38 mu m.
Example 5
(1) 0.331g of RbBr powder and 0.233g of ZrCl were taken 4 Adding the powder into a mortar, and adopting a grinding rod to grind clockwise for 5min at a grinding speed of 30r/min to fully mix the powder;
(2) Adding 5mL of acetone into a mortar, and then continuously grinding clockwise for 5min at a grinding speed of 40r/min to volatilize the acetone in the powder;
(3) Repeating the step (2) for three times, grinding for the last time until the acetone volatilizes, and drying for 2 hours at 80 ℃ to obtain the ordered vacancy leadless double perovskite micro-crystal fluorescent material, wherein the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 4 Br 2 。
Rb 2 ZrCl 4 Br 2 The excitation peak position of (2) was 284nm, the emission peak position was 477nm, and a large Stokes shift was exhibited, as shown in FIG. 5.
As can be seen from the XRD patterns in FIG. 4, rb 2 ZrCl 4 Br 2 The crystallinity is better, and the crystal structure is pure phase.
As can be seen from fig. 3, rb 2 ZrCl 4 Br 2 Is 3.778eV.
From FIG. 10, rb can be seen 2 ZrCl 4 Br 2 The fluorescence quantum yield of (2) reaches 62.8%.
From the particle size distribution statistics, rb 2 ZrCl 4 Br 2 The particle size of the particles is normally distributed, and the particle size distribution range is 0.02 mu m to 0.37 mu m.
Comparative example 1
On the basis of example 1, the powder obtained after grinding and drying was designated as powder a, without any solvent addition, and without any change in other steps and conditions.
Comparative example 2
Based on example 1, only acetone was replaced with absolute ethanol, and the other steps and conditions were unchanged, and accordingly, the powder obtained after grinding and drying was designated as powder B.
Comparative example 3
Based on example 1, except that acetone was replaced with DMF (dimethylformamide), other steps and conditions were not changed, and since the raw material powder was completely dissolved in DMF and DMF was not substantially volatilized, a dry powder could not be obtained after milling, and synthesis of the microcrystals failed.
As can be seen from the emission spectra of fig. 11, the luminescence intensity of the material obtained without the addition of the solvent in comparative example 1 and the luminescence intensity of the material obtained with the addition of the absolute ethyl alcohol in comparative example 2 are significantly lower than those obtained with the addition of acetone in example 1. In addition, the addition of DMF in comparative example 3 did not allow the synthesis of micro-crystals. From this, it is known that acetone added during the grinding process creates favorable conditions for crystallization nucleation of the microcrystals, and is a necessary solvent for preparing high crystallinity and high fluorescence emission intensity.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. An ordered vacancy leadless double perovskite micro-crystal fluorescent material is characterized in that: the chemical formula of the micro-crystal fluorescent material is Rb 2 ZrCl 6-x Br x X=0 or x=0.8 to 1.5, excitation wavelength is in the range of 200nm to 300nm, emission wavelength is in the range of 440nm to 500nm, fluorescence quantum yield is 81.2% when x=0, and fluorescence quantum yield is 85% -95% when x=0.8 to 1.5.
2. An ordered vacancy lead-free double perovskite micro-crystalline fluorescent material as claimed in claim 1 wherein: the grain size of the micron crystal fluorescent material is 0.05-0.35 mu m.
3. A method for preparing the ordered vacancy leadless double perovskite micro-crystalline fluorescent material as claimed in claim 1 or 2, wherein: the steps of the method are as follows,
the RbBr powder, the RbCl powder and the ZrCl are mixed according to the stoichiometric ratio 4 Adding the powder into a mortar, adding acetone, performing wet grinding in one direction, and removing the acetone after grinding for not less than 5min to obtain the microcrystalline fluorescent material.
4. The method for preparing ordered vacancy leadless double perovskite micro-crystal fluorescent material according to claim 3, wherein: according to ZrCl 4 The powder and acetone are 1mol: (2 mL-5 mL) acetone was added to the mill.
5. The method for preparing ordered vacancy leadless double perovskite micro-crystal fluorescent material according to claim 3, wherein: the grinding speed is 25 r/min-40 r/min, acetone is added into the mortar after the acetone volatilizes for 2 min-5 min each time, and the acetone is repeatedly added for 2-4 times.
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