CN109824086A - A kind of Na doping Cs2SbAgCl6The preparation method of Double Perovskite nano material - Google Patents
A kind of Na doping Cs2SbAgCl6The preparation method of Double Perovskite nano material Download PDFInfo
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Abstract
A kind of Na of the invention adulterates Cs2SbAgCl6The preparation method of Double Perovskite nano material belongs to semiconductor nano material preparation technical field.The specific steps are the molar ratios according to 6:2:1:3, weigh cesium chloride, silver chlorate, sodium chloride, antimony trichloride, are added in the ball grinder for the full abrading-ball that tiles after mixing, ball mill is put into after ball grinder is installed and carries out 3 hours ball millings, obtains Na:Cs2SbAgCl6Double Perovskite nano material.The advantages that present invention has mild condition, and easy to operate, the reaction time is short, easy to industrialized production, and the Na:Cs synthesized2SbAgCl6Double Perovskite nano material fluorescence quantum efficiency with higher.
Description
Technical field
The invention belongs to semiconductor nano material preparation technical fields, are related to a kind of efficient stable, and operating method simply may be used
The Na of control adulterates Cs2SbAgCl6The preparation method of Double Perovskite nano material.
Background technique
In recent years, perovskite nano material especially lead halide perovskite nano material is because of its brilliant charge-transporting
Energy and good chemical controllability, make its show one's talent in the application of solar battery, LED, laser and photodetector,
Especially in area of solar cell, photoelectric conversion efficiency can reach 20%, therefore lead halide perovskite is widely studied.
However, although lead halide perovskite has good Electronic Performance, being produced into terms of photovoltaic and photovoltaic applications
This is lower, but its stability and its its commercialized development is hampered always to human health and environmental problem.In most of states
Family expressly provided do not allow be using leaded electrical equipment, therefore the exploitation of unleaded and pure inorganic perovskite material
The toxicity of lead halide and stability problem is overcome to pay huge effort.
Published report focuses primarily upon pure inorganic CsPbX3Perovskite nano material, the perovskite material of recent research
The general formulae of material is ABX3(A=Cs2+, B=Pb2+Or Sn2+, X=Cl-,Br-,I-).One critical nature of these compounds
It is their band gap adjustability, is realized by changing the type of A, B and X.
It has recently been demonstrated that keep valence state and structural coordinates number, B1+And B3+Replace Pb2+In ABX3's
[111] it is to form Double Perovskite that void layer is generated on direction to maintain neutral charge.Replace the Tricationic knot of B area
It closes (B ') and monovalent (B ") cation and combines the A formed2B’B”X6Double Perovskite simulates ABX3Perovskite structure shows energy
Its raising to air and Moisture stability, and it is with a wide range of applications on the solar cell.But this double-deck calcium
The universal fluorescent yield of titanium ore is relatively low, the application which prevent him on photoelectric device.Therefore it is contemplated that if can improve
The fluorescent yield of Double Perovskite, and it is able to maintain its good stability, it will making this material preferably is mankind's service.
Deng in 2017 et al. successfully synthesizes Cs2SbAgCl6, band gap is indirect band gap, band gap magnitude 2.6eV, document report
Its quantum yield in road is lower, and is liquid phase synthesis, but condition required by this method is more harsh, needs in higher temperature
Under solution in carry out, in reaction heating or rate of temperature fall the particle size of final product is all had significant effect, and
The reaction time of liquid phase synthesis is generally up to 24 hours.
Summary of the invention
The technical problem to be solved by the present invention is to overcome deficiency existing for background technique, provide under a kind of normal temperature and pressure, can
The new method largely synthesized, for synthesizing Na doping Cs2SbAgCl6Double Perovskite nano material.
Technical problem of the invention solves by the following technical programs:
A kind of Na doping Cs2SbAgCl6The preparation method of Double Perovskite nano material, according to the molar ratio of 6:2:1:3,
Cesium chloride, silver chlorate, sodium chloride, antimony trichloride are weighed, is added to after mixing in the ball grinder for the full abrading-ball that tiles, ball grinder is pacified
It is put into ball mill after installing and carries out 3 hours ball millings, obtains Na:Cs2SbAgCl6Double Perovskite nano material.
Preferably, the diameter of the abrading-ball is 6mm, the rotational frequency of ball mill is 40Hz, forward and reverse alternately to transport
Row.
The utility model has the advantages that
The present invention realizes Na:Cs by mechanical lapping2SbAgCl6Synthesis, method mild condition of the invention, operation
Simply, the reaction time is short, easy to industrialized production, and the Na:Cs synthesized2SbAgCl6Double Perovskite nano material has higher
Fluorescence quantum efficiency.
Detailed description of the invention:
Fig. 1 is Cs prepared by embodiment 12SbAgCl6Double Perovskite nano material and Na:Cs2SbAgCl6The double-deck calcium titanium
The launching light spectrogram of mine nano material.
Fig. 2 is Cs prepared by embodiment 12SbAgCl6Double Perovskite nano material and Na:Cs2SbAgCl6The double-deck calcium titanium
The XRD spectrum of mine nano material.
Fig. 3 is Na:Cs prepared by embodiment 22SbAgCl6The XRD spectrum of Double Perovskite nano material.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing.
Wherein the attached figures are only used for illustrative purposes and cannot be understood as limitating the patent.
Embodiment 1: preparation Na:Cs2SbAgCl6Double Perovskite nano material
Taking tank volume is the ball grinder of 50ml, and the abrading-ball (about 15) that one layer of diameter is 6mm is filled in tiling thereto, according to
Chemical formula mole metering is than calculating m (CsCl): m (AgCl+NaCl): m (SbCl3)=2:1:1, wherein m (AgCl): m (NaCl)
=2:1 weighs the cesium chloride powder of 2mmol (0.337g), silver chlorate solid, the 0.33mmol of 0.66mmol (0.096g)
The antimony trichloride solid of (0.0132g) solid sodium chloride, 1mmol (0.228g), is put into the ball grinder of model QM-3SP04,
Tinning, which finishes to be fitted into ball grinder in ball mill pallet to hang up, draws horse, first rotates handwheel and compresses, then firmly rotates goat's horn
It tightens and ball grinder loosens and accident occurs when cap is to prevent ball mill from operating, ball grinder installs protective cover on cover, is arranged
Rotational frequency is 40Hz, using forward and reverse alternate run, the method for operation that timing is shut down is run 180 minutes, after ball milling
Drop-down horse and ball grinder are unloaded, sample and abrading-ball are poured into sieve together, ball and abrasive material are separated.It is finally recovered obtained substance
It is exactly synthetic Na:Cs2SbAgCl6Double Perovskite nano material, launching light spectrogram is as shown in Figure 1, its XRD diffraction spectra
Figure is as shown in Figure 2.Its fluorescence quantum efficiency are as follows: 24.8%.
Embodiment 2: the comparative example of Na is not mixed
Taking tank volume is the ball grinder of 50ml, and the abrading-ball (about 15) that one layer of diameter is 6mm is filled in tiling thereto, according to
Chemical formula mole metering is than calculating m (CsCl): m (AgCl): m (SbCl3)=2:1:1 weighs the cesium chloride of 2mmol (0.337g)
Powder, the silver chlorate solid of 1mmol (0.144g), 1mmol (0.228g) antimony trichloride solid, be put into model QM-3SP04
Ball grinder in, tinning finish ball grinder can be fitted into ball mill pallet hangs up draw horse, first rotate handwheel compress, then use
Ball grinder loosens and accident occurs when power rotation goat's horn is tightened and cap is to prevent ball mill from operating, and ball grinder is installed and protected on cover
Shield, setting rotational frequency are 40Hz, using forward and reverse alternate run, the method for operation that timing is shut down is run 180 minutes, ball
Drop-down horse and ball grinder are unloaded after mill, sample and abrading-ball are poured into sieve together, and ball and abrasive material are separated.It is finally recovered
To faint yellow solid powder be synthetic Cs2SbAgCl6Double Perovskite nano material, launching light spectrogram such as Fig. 1 institute
Show, XRD diffraction spectrogram is as shown in Figure 3.Its fluorescence quantum efficiency is less than 1%.
Preparation method mild condition of the invention it can be seen from the above embodiments that, easy to operate, the reaction time is short.And
The present invention is in preparation Cs2SbAgCl6Na doping, after being doped with sodium, fluorescence volume have also been carried out when Double Perovskite nano material
Sub- efficiency, which has, to be obviously improved.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (2)
1. a kind of Na adulterates Cs2SbAgCl6The preparation method of Double Perovskite nano material claims according to the molar ratio of 6:2:1:3
Cesium chloride, silver chlorate, sodium chloride, antimony trichloride are taken, is added to after mixing in the ball grinder for the full abrading-ball that tiles, ball grinder is installed
It is put into ball mill after good and carries out 3 hours ball millings, obtains Na:Cs2SbAgCl6Double Perovskite nano material.
2. a kind of Na according to claim 1 adulterates Cs2SbAgCl6The preparation method of Double Perovskite nano material, it is special
Sign is that the diameter of the abrading-ball is 6mm, and the rotational frequency of ball mill is 40Hz, forward and reverse alternate run.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110938428A (en) * | 2019-12-03 | 2020-03-31 | 吉林大学 | High-efficiency synthetic Cs2AgCl3Method for preparing all-inorganic non-lead perovskite |
| CN111073637A (en) * | 2019-12-03 | 2020-04-28 | 北京理工大学 | Zero-dimensional lead-free perovskite fluorescent material, and preparation and application thereof |
| CN111139068A (en) * | 2019-12-03 | 2020-05-12 | 北京理工大学 | Zero-dimensional lead-free perovskite Cs3Cu2X5Preparation method and application of |
| CN113697855A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院上海硅酸盐研究所 | Cu-doped double perovskite material and preparation method thereof |
| CN116790247A (en) * | 2023-04-20 | 2023-09-22 | 安顺学院 | Preparation method of all-inorganic lead-free halide multicolor luminescent fluorescent powder, product and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10927013B2 (en) * | 2015-09-02 | 2021-02-23 | Oxford University Innovation Limited | Double perovskite |
| WO2018231909A1 (en) * | 2017-06-13 | 2018-12-20 | Board Of Trustees Of Michigan State University | Method for fabricating epitaxial halide perovskite films and devices |
| CN108659827B (en) * | 2018-06-15 | 2020-07-10 | 华中科技大学 | Near ultraviolet excited double perovskite single-substrate white light fluorescent material and preparation and application thereof |
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- 2019-04-04 CN CN201910268600.9A patent/CN109824086B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110938428A (en) * | 2019-12-03 | 2020-03-31 | 吉林大学 | High-efficiency synthetic Cs2AgCl3Method for preparing all-inorganic non-lead perovskite |
| CN111073637A (en) * | 2019-12-03 | 2020-04-28 | 北京理工大学 | Zero-dimensional lead-free perovskite fluorescent material, and preparation and application thereof |
| CN111139068A (en) * | 2019-12-03 | 2020-05-12 | 北京理工大学 | Zero-dimensional lead-free perovskite Cs3Cu2X5Preparation method and application of |
| CN110938428B (en) * | 2019-12-03 | 2021-08-31 | 吉林大学 | High-efficiency synthetic Cs2AgCl3Method for preparing all-inorganic non-lead perovskite |
| CN111073637B (en) * | 2019-12-03 | 2021-09-07 | 北京理工大学 | Zero-dimensional lead-free perovskite fluorescent material, and preparation and application thereof |
| CN113697855A (en) * | 2020-05-20 | 2021-11-26 | 中国科学院上海硅酸盐研究所 | Cu-doped double perovskite material and preparation method thereof |
| CN113697855B (en) * | 2020-05-20 | 2022-07-12 | 中国科学院上海硅酸盐研究所 | Cu-doped double perovskite material and preparation method thereof |
| CN116790247A (en) * | 2023-04-20 | 2023-09-22 | 安顺学院 | Preparation method of all-inorganic lead-free halide multicolor luminescent fluorescent powder, product and application thereof |
| CN116790247B (en) * | 2023-04-20 | 2024-06-11 | 安顺学院 | Preparation method of all-inorganic lead-free halide multicolor luminescent fluorescent powder, product and application thereof |
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