CN117026375A - Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material and preparation method and application thereof - Google Patents
Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material and preparation method and application thereof Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 19
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
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- 230000035515 penetration Effects 0.000 description 1
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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- C09K11/7773—Halogenides with alkali or alkaline earth metal
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
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Abstract
The application relates to the technical field of near infrared luminescence, in particular to a lanthanide ion doped Cs 2 NaYCl 6 Perovskite material, preparation method and application thereof, and CsCl, naCl, YCl is prepared by adopting hydrothermal reaction synthesis method 3 ·6H 2 O，Er(CH 3 COO) 3 ·4H 2 O or Nd (CH) 3 COO) 3 ·4H 2 Dissolving O in concentrated hydrochloric acid, heating the mixed solution at high temperature, cooling to room temperature to precipitate crystals, and washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ The safety of the monocrystal during the synthesis process is greatly improved, and the monocrystal can be also provided with large scaleThe die synthesis has the potential of large-scale preparation, greatly improves the near infrared luminous efficiency of the LED, reduces the manufacturing cost, can be used for large-scale commercial manufacturing, and has huge application prospect in night vision and nondestructive detection.
Description
Technical Field
The application relates to the technical field of near infrared luminescence, in particular to a lanthanide ion doped Cs 2 NaYCl 6 Perovskite material, and a preparation method and application thereof.
Background
The near infrared light source has the advantages of low thermal effect, no damage and large penetration depth, and development of the high-efficiency near infrared light source is always the research key point in the current field. Lead halide double perovskite has excellent optical properties and can be an excellent candidate material for near infrared emission, but the poor toxicity and stability are great barriers for further industrial application.
The double perovskite with little pollution to the environment is an excellent substitute for the lead halide double perovskite, the photoelectric performance of which is equivalent to that of the lead halide double perovskite, however, the double perovskite generally shows poor optical performance because of indirect band gap or parity forbidden transition, and in order to improve the luminous intensity of the double perovskite, metal ion doping has proven to be a viable strategy and has achieved remarkable achievement in the research of visible light. Such as Cs 2 AgInCl 6 :Yb 3+ And Cs 2 (Na/Ag)InCl 6 :Ho 3+ ) But it is hardly applicable due to its poor emission efficiency. The most advanced research shows that the introduction of metal ion sensitizers into host matrices is a viable approach to improve the near infrared luminous efficiency of double perovskite. For example, bi 3+ /Er 3+ And Bi (Bi) 3+ /Yb 3+ Co-doping Cs 2 AgInCl 6 Near infrared emission intensities of (a) are respectively about Er 3+ And Yb 3+ Singly mix Cs 2 AgInCl 6 45 and 27 times of (c). At the same time Sb 3+ And Te (Te) 4+ It has also been demonstrated to enhance the lanthanoid Ln by energy transfer 3+ Ideal sensitizers for ion emission.
Although preliminary progress has been made, co-doping strategies involve complex interactions between the various dopants, which prevent their independent role in near infrared emission from being clearly identified. Furthermore, their further use is severely limited by the lower near infrared emission efficiency and the shorter excitation wavelength (< 420 nm). Thus, there is an urgent need for an ideal host matrix to address the problems faced in the double perovskite with near infrared emissions.
Disclosure of Invention
The application aims to provide the lanthanide ion doped Cs which has the advantages of simple process, low cost, environmental protection, no toxicity and excellent performance 2 NaYCl 6 Perovskite material, and a preparation method and application thereof.
To achieve the above object, the present application provides a lanthanide ion doped Cs 2 NaYCl 6 A method for preparing a perovskite material comprising the steps of:
obtaining raw materials, and dissolving the raw materials in concentrated hydrochloric acid to obtain a mixed solution;
heating the mixed solution at a high temperature;
cooling the mixed solution to room temperature after high-temperature heating, and separating out crystals;
washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ And (3) single crystals.
Wherein, obtain the raw materials, and dissolve the raw materials in concentrated hydrochloric acid, obtain mixed solution, the method still includes:
the raw material is CsCl, naCl, YCl 3 · 6 H 2 O and Er (CH) 3 COO) 3 ·4H 2 O。
Wherein, obtain the raw materials, and dissolve the raw materials in concentrated hydrochloric acid, obtain mixed solution, the method still includes:
the raw material is CsCl, naCl, YCl 3 · 6 H 2 O and Nd (CH) 3 COO) 3 ·4H 2 O。
Wherein the mixed solution is heated at a high temperature, the method further comprising:
placing the mixed solution into a polytetrafluoroethylene lining;
placing the lining into a reaction kettle;
the reaction kettle is heated at a high temperature of 180 ℃ for 10 hours.
Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material, cs doped by adopting lanthanide ion 2 NaYCl 6 Perovskite material preparationThe preparation method is used for preparing the product.
Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material application, the lanthanide ion doped Cs 2 NaYCl 6 Perovskite materials are used as near infrared luminescent materials.
Wherein the lanthanide ion doped Cs 2 NaYCl 6 The perovskite material is used for preparing an LED chip and a near infrared LED lamp thereof.
The application relates to a lanthanide ion doped Cs 2 NaYCl 6 Perovskite material, preparation method and application thereof, and CsCl, naCl, YCl is synthesized by adopting hydrothermal reaction 3 · 6 H 2 O，Er(CH 3 COO) 3 ·4H 2 O or Nd (CH) 3 COO) 3 ·4H 2 Dissolving O in concentrated hydrochloric acid, heating the mixed solution at high temperature, cooling to room temperature to precipitate crystals, and washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ Compared with the prior art, the monocrystalline silicon material has the following beneficial effects:
the used synthetic materials are environment-friendly materials, and toxic heavy metals (such as lead, cadmium, mercury and the like) are not contained, so that the near infrared LED has better environment inclusion, can be applied in multiple fields, and does not pollute the environment;
provides a hydrothermal reaction method for synthesizing Cs 2 NaYCl 6 Perovskite system doped with Er 3+ 、Nd 3+ The safety of the powder in the synthesis process is greatly improved, and the powder can be synthesized in a large scale, so that the powder has the potential of large-scale preparation;
based on Cs 2 NaYCl 6 Perovskite system doped with Er 3+ 、Nd 3+ The near infrared LED has high near infrared luminous efficiency of 93+/-2% and 51+/-3% under excitation of 520nm and 580nm respectively, greatly reduces energy loss, improves the utilization rate of energy, has good energy-saving effect and accords with the current generation development;
the near infrared luminous efficiency of the LED is greatly improved, the manufacturing cost is reduced, and the LED can be manufactured in a large scale, and has a huge application prospect in night vision and nondestructive detection.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a graph of Cs of the present application 2 NaYCl 6 Er-doped 3+ Is a graph of the luminescence mechanism of (a).
FIG. 2 is a graph of Cs of the present application 2 NaYCl 6 Nd-doped 3+ Is a graph of the luminescence mechanism of (a).
FIG. 3 is a graph of Cs of the present application 2 NaYCl 6 Er-doped 3+ Example diagrams of LED applications.
FIG. 4 is a graph of Cs of the present application 2 NaYCl 6 Nd-doped 3+ Example diagrams of LED applications.
FIG. 5 is a lanthanide ion doped Cs of the present application 2 NaYCl 6 Perovskite material is used for preparing the flow chart of the near infrared LED lamp.
FIG. 6 is a lanthanide ion doped Cs of the present application 2 NaYCl 6 A step diagram of a perovskite material preparation method.
Detailed Description
The following detailed description of embodiments of the application, examples of which are illustrated in the accompanying drawings and, by way of example, are intended to be illustrative, and not to be construed as limiting, of the application.
Referring to fig. 1-6, fig. 1 shows Cs according to the present application 2 NaYCl 6 Er-doped 3+ Is a graph of the luminescence mechanism of (a). FIG. 2 is a graph of Cs of the present application 2 NaYCl 6 Nd-doped 3+ Is a graph of the luminescence mechanism of (a). FIG. 3 is a graph of Cs of the present application 2 NaYCl 6 Er-doped 3+ Example diagrams of LED applications. FIG. 4 is a graph of Cs of the present application 2 NaYCl 6 Nd-doped 3+ Example diagrams of LED applications. FIG. 5 is a lanthanide ion doped Cs of the present application 2 NaYCl 6 Perovskite material is used for preparing the flow chart of the near infrared LED lamp. FIG. 6 is a lanthanide ion doped Cs of the present application 2 NaYCl 6 Steps of perovskite material preparation methodAnd (7) carrying out a step diagram.
The application provides a lanthanide ion doped Cs 2 NaYCl 6 The preparation method of the perovskite material comprises the following steps: the method comprises the following steps:
s101: obtaining raw materials, and dissolving the raw materials in concentrated hydrochloric acid to obtain a mixed solution;
s102: heating the mixed solution at a high temperature;
s103: cooling the mixed solution to room temperature after high-temperature heating, and separating out crystals;
s104: washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ And (3) single crystals.
Specifically, the hydrothermal reaction synthesis method is carried out according to the following operation: will CsCl, naCl, YCl 3 ·6H 2 O，Er(CH 3 COO) 3 ·4H 2 O or Nd (CH) 3 COO) 3 ·4H 2 O is dissolved in concentrated hydrochloric acid, wherein CsCl, naCl, YCl 3 · 6 H 2 O，Er(CH 3 COO) 3 ·4H 2 O or Nd (CH) 3 COO) 3 ·4H 2 O and concentrated hydrochloric acid with the dosage of 2mmol,1mmol, 0.25mmol or 0.3mmol and 4ml respectively, putting the mixed solution into a polytetrafluoroethylene lining, then putting the lining into a reaction kettle, heating the reaction kettle at a high temperature of 180 ℃ for 10 hours, cooling at 4 ℃/h, precipitating crystals at room temperature, and washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ Experimental study shows that the application synthesizes Er doped through hydrothermal reaction 3+ Cs of (2) 2 NaYCl 6 Rare earth-based double perovskite of (2) is obtained from Er 3+ Strong and multi-wavelength near infrared emission of 4f-4f conversion and Er under green (520 nm) excitation 3+ Doped Cs 2 NaYCl 6 Exhibits 93+ -2% efficient PLQE in the near infrared-II region (1430-1600 nm), which makes it of great application potential in low-loss optical communication, and photophysical mechanism shows from self-trapped exciton (STE) to Er 3+ With efficient energy transfer (E-T) and phaseAdjacent Er 3+ A significant cross relaxation process (C-R) between (and (C-R) to enable Er to 3+ Doped Cs 2 NaYCl 6 Has high near infrared emission, and in addition, in Cs 2 NaYCl 6 Also incorporate Nd 3+ Also has high efficiency near infrared emission.
Compared with the prior art, the application has the following beneficial effects:
the synthetic materials used in the application are environment-friendly materials, and have no toxic heavy metals (such as lead, cadmium, mercury and the like), so that the near-infrared LED has better environment inclusion, can be applied in multiple fields, and does not pollute the environment;
the application provides a hydrothermal reaction method for synthesizing Cs 2 NaYCl 6 Perovskite system doped with Er 3+ 、Nd 3+ The safety of the powder in the synthesis process is greatly improved, and the powder can be synthesized in a large scale, so that the powder has the potential of large-scale preparation;
the application is based on Cs 2 NaYCl 6 Perovskite system doped with Er 3+ 、Nd 3+ The near infrared LED has high near infrared luminous efficiency of 93+/-2% and 51+/-3% under excitation of 520nm and 580nm respectively, greatly reduces energy loss, improves the utilization rate of energy, has good energy-saving effect and accords with the current generation development;
the application greatly improves the near infrared luminous efficiency of the LED, reduces the manufacturing cost, can be manufactured in a large scale and has huge application prospect in night vision and nondestructive detection.
The application provides a lanthanide ion doped Cs 2 NaYCl 6 Perovskite material, cs doped by adopting lanthanide ion 2 NaYCl 6 The perovskite material is prepared by a preparation method.
Specifically, the lanthanide ion is Er 3+ Or Nd 3+ The lanthanide ion is Er 3+ Or Nd 3+ When the strongest emission is excited directly at 520nm or 580 nm.
The application provides a lanthanide ion doped Cs 2 NaYCl 6 Perovskite materialAnd (5) material application.
Specifically, the resulting lanthanide ion doped Cs 2 NaYCl 6 Perovskite material used as near infrared luminescent material, the lanthanide ion doped Cs 2 NaYCl 6 In preparing LED chips and near infrared LED lamps thereof from perovskite materials, cs is prepared 2 NaYCl 6 Er-doped 3+ Powder or Nd 3+ And uniformly coating the powder on an LED chip with the wavelength of 520nm or 580nm, and packaging to obtain the near infrared LED lamp.
Example 1
Preparation of Cs 2 NaYCl 6 Perovskite system doped with Er 3+ Powder
2mmol of CsCl,1mmol of NaCl,1mmolYCl 3 ·6H 2 O also has 0.25mmole Er (CH 3 COO) 3 ·4H 2 O is dissolved in 4ml of concentrated hydrochloric acid, the mixed solution is put into a 25ml polytetrafluoroethylene lining, then the lining is put into a reaction kettle and is screwed up, the reaction kettle is heated for 10 hours at the high temperature of 180 ℃, then the temperature is reduced to room temperature at 4 ℃/h, crystals can be separated out, and the crystals are washed three times by ethanol, thus obtaining Cs 2 NaYCl 6 Er-doped 3+ And (3) single crystals.
FIG. 1 shows the Cs obtained in example 1 2 NaYCl 6 Er-doped 3+ Is a luminous mechanism diagram of (a): under high energy excitation (e.g., 266 nm), due to Cs 2 NaYCl 6 The well-established electron-phonon coupling, the photo-generated exciton is rapidly trapped by the self-trapping exciton. Then, when the generated STEs relax to the ground state, it can be seen that the STEs come from [ YCl ] 6 ] 3- The sky blue emission of the clusters. At the same time, some electrons are transferred to Er in the doped sample by E-T 3+ . Thus, one can see Er 3+ The f-f conversion of (c) produces a multi-wavelength emission. Furthermore, er 3+ The strongest emission of (2) can be directly excited at 520nm, which is a clear quantum clipping process as evidenced by the strong absorption of PLE spectra and f-f conversions, resulting in near infrared emissions with a near-hundred percent quantum efficiency. In particular, adjacent Er 3+ The ions have obvious C-R, more particularly a quantumThe clipping process promotes electron groups of 4I13/2 energy level, thereby realizing Er in the near infrared-II region 3+ The efficient PLQE of the emission, which indicates that the spin orbitals here come from the interaction and the effect of the magnetic coupling.
Example 2
Preparation of Cs 2 NaYCl 6 Nd-doped perovskite system 3+ Powder
2mmol of CsCl,1mmol of NaCl,1mmolYCl 3 ·6H 2 O also has 0.3mmolNd (CH) 3 COO) 3 ·4H 2 O is dissolved in 4ml of concentrated hydrochloric acid, the mixed solution is put into a 25ml polytetrafluoroethylene lining, then the lining is put into a reaction kettle and is screwed up, the reaction kettle is heated for 10 hours at 180 ℃, then the temperature is reduced to room temperature at 4 ℃/h, crystals can be separated out, and the crystals are washed three times by ethanol, thus obtaining Cs 2 NaYCl 6 Nd-doped 3+ And (3) single crystals.
FIG. 2 shows the Cs obtained in example 2 2 NaYCl 6 Nd-doped 3+ Luminescence mechanism diagram of ion, its luminescence mechanism and Cs 2 NaYCl 6 Er-doped 3+ Similarly, the quantum clipping process is not existed, and the description is omitted.
Application example
Cs doped with lanthanide ions obtained in example 1 and example 2 2 NaYCl 6 Perovskite materials corresponding near infrared LED lamps were prepared respectively with reference to fig. 5.
FIG. 3 shows Cs 2 NaYCl 6 Er-doped 3+ The manufactured near infrared LED irradiates a near infrared image graph obtained by the hand, so that the LED can be clearly seen to easily penetrate the finger (about 15 mm) and the wrist (about 40 mm) of a person, and the vein distribution of the person is clearly visible.
FIG. 4 shows Cs under visible light 2 NaYCl 6 Nd-doped 3+ And a photo of flowers and grass is taken under the manufactured near infrared LED. When the NIR-LED is off, the NIR camera does not take anything; while when the NIR-LED is on, black and white images of grass and flowers are recorded by the NIR camera.
The foregoing disclosure is only illustrative of one or more preferred embodiments of the present application, and it is not intended to limit the scope of the claims hereof, as persons of ordinary skill in the art will understand that all or part of the processes for practicing the embodiments described herein may be practiced with equivalent variations in the claims, which are within the scope of the application.
Claims (7)
1. Lanthanide ion doped Cs 2 NaYCl 6 The preparation method of the perovskite material is characterized by comprising the following steps of:
obtaining raw materials, and dissolving the raw materials in concentrated hydrochloric acid to obtain a mixed solution;
heating the mixed solution at a high temperature;
cooling the mixed solution to room temperature after high-temperature heating, and separating out crystals;
washing the crystals with ethanol to obtain Cs 2 NaYCl 6 Er-doped 3+ Or Nd 3+ And (3) single crystals.
2. Lanthanide ion doped Cs of claim 1 2 NaYCl 6 A method for producing a perovskite material, characterized by obtaining a raw material and dissolving the raw material in concentrated hydrochloric acid to obtain a mixed solution, the method further comprising:
the raw material is CsCl, naCl, YCl 3 ·6H 2 O and Er (CH) 3 COO) 3 ·4H 2 O。
3. Lanthanide ion doped Cs of claim 1 2 NaYCl 6 A method for producing a perovskite material, characterized by obtaining a raw material and dissolving the raw material in concentrated hydrochloric acid to obtain a mixed solution, the method further comprising:
the raw material is CsCl, naCl, YCl 3 · 6 H 2 O and Nd (CH) 3 COO) 3 ·4H 2 O。
4. Lanthanide ion doped Cs of claim 1 2 NaYCl 6 A method for producing a perovskite material, characterized in that the mixed solution is heated at a high temperature, the method further comprising:
placing the mixed solution into a polytetrafluoroethylene lining;
placing the lining into a reaction kettle;
the reaction kettle is heated at a high temperature of 180 ℃ for 10 hours.
5. Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material doped with lanthanide ions as defined in claim 1 2 NaYCl 6 The perovskite material is prepared by a preparation method.
6. Lanthanide ion doped Cs 2 NaYCl 6 Perovskite material application, suitable for lanthanide ion doped Cs according to claim 5 2 NaYCl 6 A perovskite material, characterized in that,
the lanthanide ion doped Cs 2 NaYCl 6 Perovskite materials are used as near infrared luminescent materials.
7. The lanthanide ion-doped Cs of claim 6 2 NaYCl 6 A perovskite material, characterized in that,
the lanthanide ion doped Cs 2 NaYCl 6 The perovskite material is used for preparing an LED chip and a near infrared LED lamp thereof.
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