CN113201329A - Perovskite type fluoride luminescent material and preparation method thereof - Google Patents
Perovskite type fluoride luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a perovskite fluoride luminescent material, the chemical composition of which is KCu(1‑x)F3:xMn4+Wherein x is the mole percentage coefficient of the doped manganese ions relative to the copper ions and is 0<x is less than or equal to 0.2; the preparation method comprises the following steps: (1) weighing 10-20 parts of hydrofluoric acid, 60-80 parts of potassium hexafluoromanganate or 50-75 parts of potassium permanganate, 60-90 parts of copper oxide or 70-90 parts of copper carbonate, 50-85 parts of potassium fluoride or 75-95 parts of potassium bifluoride; (2) sequentially adding potassium hexafluoromanganate or potassium permanganate, copper oxide or copper carbonate and potassium fluoride or potassium bifluoride into hydrofluoric acid, and magnetically stirring to obtain a precipitate; (3) washing the precipitate with ethanol, and drying. The invention uses positive quadrivalent transition metal Mn4+The perovskite fluoride is taken as a substrate to prepare the luminescent material with good thermal stability as a luminescent center.
Description
Technical Field
The invention relates to the technical field of inorganic functional materials, in particular to a perovskite fluoride luminescent material and a preparation method thereof.
Background
Perovskite compounds were discovered by the german mineralist Gustav Rose in 1839, while the russian mineralist l.a.perovski, who abbreviated the structural formula of the compound as ABX, was the first person to describe the perovskite crystal structure3. Initially, perovskite was referred to as CaTiO3Then expanded to all of the groups with CaTiO3Compounds with similar structure and different chemical compositions. Perovskite-type compound (ABX)3) It is common in nature that the properties of a compound are altered when the a or B ion is substituted, but the crystal structure remains unchanged. The perovskite type inorganic compound has the advantages of stable crystal structure, excellent photoelectric property, various synthesis approaches, narrow emission peak and adjustable forbidden band width when being applied to the field of luminescence, and low cost, thereby being concerned.
The white light LED is a new generation light source in the 21 st century because of its advantages of low working voltage, high luminous efficiency, long service life, small size, good stability, environmental friendliness, etc. At present, three methods for realizing white light by using an LED are mainly used, the first method is to combine light emission by using an LED chip which emits red, green and blue tricolor light to synthesize the white light, but the cost is high, the packaging difficulty is high, the stability is poor, and a control circuit is complex; the second one is produced by combining a near ultraviolet LED chip and tricolor fluorescent powder, but the luminous efficiency is low, the temperature stability of the fluorescent powder is not high, the ultraviolet light leakage danger exists, and the wide application is difficult; the third is to use a blue LED chip to excite yellow fluorescent powder, and the combined approach is most widely applied, but the color rendering index is low, the color temperature is high, and the special illumination requirements are difficult to meet.
Therefore, it is of great significance to develop a red luminescent material with high-efficiency blue light absorption, excellent thermal stability and simple preparation.
Disclosure of Invention
In view of the above, the present invention provides a perovskite-type fluoride luminescent material and a preparation method thereof, wherein a positive tetravalent transition metal manganese ion is used as a luminescent center, and a substrate is subjected to positive tetravalent manganese ion pairThe substitution of the lattice site of the medium and positive divalent copper ions realizes that the chemical composition is KCu(1-x)F3:xMn4+Absorption in the ultraviolet region, blue region and emission in the red region, and Mn4+Does not change the lattice structure of the host material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a perovskite fluoride luminescent material has a chemical composition of KCu(1-x)F3:xMn4+(ii) a Wherein x is the mole percentage coefficient of the doped manganese ions relative to the copper ions, and 0<x≤0.2。
The invention has the beneficial effect that the applicant discovers Mn through a large amount of experimental researches4+Occurring in octahedral crystal fields2Eg→4A2gThe energy level transition of the red light can form red narrow-band emission, the red light can be used for preparing warm white light LEDs, and the red light also has strong broadband absorption in an ultraviolet light region and a blue light region, which respectively correspond to the ultraviolet light region and the blue light region4A2g→4T1gTransition and4A2g→4T2gthe prepared luminescent material has good stability, high color purity and small light decay. Therefore, the perovskite fluoride has the characteristics of stable crystal structure, high melting point, wide energy band gap, various structures and appearances and the like, and Mn4+And the wide blue light excitation and narrow red light emission characteristics are shown in an octahedral crystal field.
Therefore, the invention uses the positive quadrivalent transition metal Mn4+As a luminescent center, fluoride ions are taken as anions, perovskite type fluoride is taken as a substrate, and the luminescent material with good thermal stability is prepared, and the chemical composition of the luminescent material is KCu(1-x)F3:xMn4+. The negative ions of the substrate material are fluorine ions, the lattice structure is perovskite type, namely the lattice structure unit of the substrate is a cube, the potassium ions occupy the vertex lattice position of the cube, the copper ions occupy the center lattice position of the cube, and the fluorine ions occupy the face center lattice position of the cube.
Furthermore, the perovskite fluoride luminescent material is prepared by reacting 10-20 parts by weight of hydrofluoric acid, 60-80 parts by weight of potassium hexafluoromanganate or 50-75 parts by weight of potassium permanganate, 60-90 parts by weight of copper oxide or 70-90 parts by weight of copper carbonate, and 50-85 parts by weight of potassium fluoride or 75-95 parts by weight of potassium bifluoride.
The further technical scheme has the advantages that hydrofluoric acid provides a fluorine source required by an acidic environment compound required by the reaction, potassium hexafluoromanganate or potassium permanganate provides a manganese source, copper oxide or copper carbonate provides a copper source, and potassium fluoride or potassium bifluoride provides a potassium source and a fluorine source. The reaction equation is as follows: CuO + KF +2HF ═ H2O+KCuF3；KCuF3+xK2MnF6＝KCu(1-x)MnxF3。
A preparation method of a perovskite fluoride luminescent material specifically comprises the following steps:
(1) weighing 10-20 parts of hydrofluoric acid, 60-80 parts of potassium hexafluoromanganate or 50-75 parts of potassium permanganate, 60-90 parts of copper oxide or 70-90 parts of copper carbonate, 50-85 parts of potassium fluoride or 75-95 parts of potassium bifluoride;
(2) sequentially adding potassium hexafluoromanganate or potassium permanganate, copper oxide or copper carbonate and potassium fluoride or potassium bifluoride into hydrofluoric acid, and magnetically stirring to obtain a precipitate;
(3) and washing the precipitate with ethanol, and drying to obtain the perovskite fluoride luminescent material.
The invention has the advantages of wide raw material source, simple operation and short reaction period, and can be prepared at room temperature.
Further, in the step (2), the temperature of magnetic stirring is 18-25 ℃, the speed is 400-.
The further technical scheme has the beneficial effects that the added raw materials can be uniformly mixed by magnetic stirring, so that the reaction can be carried out more fully; the reaction temperature of 18-25 ℃ and the reaction time of 10-15h effectively avoid other impurities caused by overhigh reaction temperature and overlong reaction time or insufficient reaction temperature and time; the rotating speed of 400-600r/min ensures that all the raw materials are fully mixed, and simultaneously avoids liquid splashing.
Further, in the step (3), the number of washing with ethanol is 4 to 6.
The further technical scheme has the advantages that the ethanol washing can disperse precipitates, so that impurities in the precipitates can be removed conveniently, and the drying time is shortened; 4-6 times of washing avoids the problems of impurity of products caused by insufficient washing or excessive loss of precipitation.
Further, in the step (3), the drying temperature is 60-90 ℃ and the drying time is 24-48 h.
The beneficial effect of adopting the further technical scheme is that the drying in the vacuum drying oven can firstly dry the product in a short time, which is convenient for the subsequent analysis and test, and secondly can avoid the loss and pollution of the product caused by the blowing or moving of the powder sample by the flowing air. The drying temperature of 60-90 ℃ and the drying time of 24-48h effectively avoid the influence of insufficient temperature and time on the analysis and test after the product contains moisture or other impurities are introduced due to overhigh temperature and overlong time.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the perovskite fluoride luminescent material has uniform particles, clear edges and corners, smooth surface and irregular polygonal sheet shape, and starts thermal decomposition at the high temperature of about 560 ℃.
2. The perovskite fluoride luminescent material of the invention generates a series of narrow-band red light emission peaks under the excitation of 450nm blue light, the emission peak is positioned in the wavelength range of 590-650nm, the half-peak width is not more than 2nm, the emission peaks are respectively positioned at 598nm, 609nm, 613nm, 631nm and 647nm, the strongest emission peak is positioned at 631nm, and the red light emission intensity can still keep more than 50% of the room temperature when the working temperature is 160 ℃.
3. The perovskite fluoride luminescent material shows strong absorption bands in the ultraviolet light range of 300-400nm and the blue light range of 400-520nm, and the half-peak width of the blue light absorption band is about 50 nm.
Drawings
FIG. 1 is a view showing a perovskite type fluoride luminescent material KCu in example 10.95F3:0.05Mn4+XRD diffractogram of (a);
FIG. 2 is a view showing a perovskite type fluoride luminescent material KCu in example 10.95F3:0.05Mn4+SEM picture of (1);
FIG. 3 shows a perovskite-type fluoride emission material KCu in example 10.95F3:0.05Mn4+Excitation and emission spectra at room temperature;
FIG. 4 is a view showing a perovskite type fluoride luminescent material KCuF of example 33:Mn4+A variable temperature spectrogram at 20-200 deg.C;
FIG. 5 is a view showing a perovskite type fluoride luminescent material KCu of example 30.95F3:0.05Mn4+A linear relationship diagram of the thermal stability activation energy of (1).
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium hexafluoromanganate, 0.2g of copper oxide and 0.174g of potassium fluoride;
(2) adding hydrofluoric acid into a plastic test tube with a stirrer, sequentially adding potassium hexafluoromanganate and copper oxide at the temperature of 18 ℃, magnetically stirring at a constant speed of 400r/min for 15min, adding potassium fluoride, and stirring for 10h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, drying in an oven at 80 deg.C for 24 hr to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
FIG. 1 is a view showing a perovskite type fluoride luminescent material KCu in example 10.95F3:0.05Mn4+XRD diffractogram of (a). As can be seen from FIG. 1, the diffraction peak and the matrix KCuF3The diffraction peaks of the standard card (JCPDS No. 73-0233) of (A) are completely corresponding, which indicates that the synthesized sample has a single crystal phase and the luminescence center Mn4+Does not change the lattice structure of the substrate.
FIG. 2 is a view showing a perovskite type fluoride luminescent material KCu in example 10.95F3:0.05Mn4+SEM image of (d). As can be seen from fig. 2, the sample surface was smooth, the crystallinity was good, and the particles were in the form of irregular polygonal flakes.
FIG. 3 shows a perovskite-type fluoride emission material KCu in example 10.95F3:0.05Mn4+Excitation spectrum and emission spectrum at room temperature. As can be seen from FIG. 3, two distinct broadband excitation peaks can be observed in the wavelength range of 300-500 nm; under the excitation of blue light at 450nm, a series of sharp narrow-band emission peaks can be observed in the wavelength range of 590-650nm, the half-peak width of the emission peaks does not exceed 2nm, and the strongest emission is located at 631 nm.
Example 2
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium hexafluoromanganate, 0.5525g of copper carbonate and 0.174g of potassium fluoride;
(2) adding hydrofluoric acid into a plastic test tube with a stirrer, sequentially adding potassium hexafluoromanganate and copper carbonate at the temperature of 20 ℃, magnetically stirring at a constant speed of 500r/min for 20min, adding potassium fluoride, and stirring for 12h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, and drying in an oven at 80 deg.C for 36h to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
Example 3
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium hexafluoromanganate, 0.2g of copper oxide and 0.234g of potassium bifluoride;
(2) adding hydrofluoric acid into a plastic test tube with a stirrer, sequentially adding potassium hexafluoromanganate and copper oxide at the temperature of 22 ℃, magnetically stirring at a constant speed of 600r/min for 15min, adding potassium bifluoride, and stirring for 12h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, drying in an oven at 80 deg.C for 48h to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
FIG. 4 is a view showing a perovskite type fluoride luminescent material KCuF of example 33:Mn4+A variable temperature spectrogram in the range of 20-200 ℃. As can be seen from FIG. 4, when the operating temperature is 160 ℃, the luminous intensity of the material still maintains more than 50% of that of the material at room temperature; in addition, when the working temperature is lower than 140 ℃, the luminous intensity of the material shows a slow descending trend along with the increase of the working temperature, which indicates that the luminous material has better thermal stability.
FIG. 5 is a view showing a perovskite type fluoride luminescent material KCu of example 30.95F3:0.05Mn4+A linear relationship diagram of the thermal stability activation energy of (1). As can be seen from FIG. 5, the calculation result shows that the thermal stability activation energy of the product is 0.6473eV, which proves that the luminescent material has good thermal stability.
Example 4
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium hexafluoromanganate, 0.5525g of copper carbonate and 0.234g of potassium bifluoride;
(2) adding hydrofluoric acid into a plastic test tube with a stirrer, sequentially adding potassium hexafluoromanganate and copper carbonate at the temperature of 22 ℃, magnetically stirring at a constant speed of 400r/min for 20min, adding potassium bifluoride, and stirring for 15h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, and drying in an oven at 80 deg.C for 36h to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
Example 5
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium permanganate, 0.2g of copper oxide and 0.234g of potassium bifluoride;
(2) adding hydrofluoric acid into a plastic test tube provided with a stirrer, sequentially adding potassium permanganate and potassium bifluoride at the temperature of 24 ℃, magnetically stirring at a constant speed of 400r/min for 15min, adding potassium fluoride, and stirring for 12h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, drying in an oven at 80 deg.C for 48h to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
Example 6
Perovskite type fluoride luminescent material KCu0.95F3:0.05Mn4+The preparation method specifically comprises the following steps:
(1) weighing 4mL of hydrofluoric acid, 0.0031g of potassium hexafluoromanganate, 0.5525g of copper carbonate and 0.234g of potassium bifluoride;
(2) adding hydrofluoric acid into a plastic test tube with a stirrer, sequentially adding potassium hexafluoromanganate and copper carbonate at 25 ℃, magnetically stirring at a constant speed of 500r/min for 20min, adding potassium bifluoride, and stirring for 15h to obtain a precipitate;
(3) washing the precipitate with ethanol for 6 times, and drying in an oven at 80 deg.C for 36h to obtain perovskite fluoride luminescent material KCu0.95F3:0.05Mn4+。
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A perovskite fluoride luminescent material is characterized in that the chemical composition is KCu(1-x)F3:xMn4+；
Wherein x is a mole percentage coefficient of the doped manganese ions relative to the copper ions, and x is more than 0 and less than or equal to 0.2.
2. The perovskite fluoride luminescent material as claimed in claim 1, wherein the perovskite fluoride luminescent material is prepared by reaction of 10-20 parts by weight of hydrofluoric acid, 60-80 parts by weight of potassium hexafluoromanganate or 50-75 parts by weight of potassium permanganate, 60-90 parts by weight of copper oxide or 70-90 parts by weight of copper carbonate, 50-85 parts by weight of potassium fluoride or 75-95 parts by weight of potassium bifluoride.
3. The preparation method of the perovskite fluoride luminescent material is characterized by comprising the following steps:
(1) weighing 10-20 parts of hydrofluoric acid, 60-80 parts of potassium hexafluoromanganate or 50-75 parts of potassium permanganate, 60-90 parts of copper oxide or 70-90 parts of copper carbonate, 50-85 parts of potassium fluoride or 75-95 parts of potassium bifluoride;
(2) sequentially adding potassium hexafluoromanganate or potassium permanganate, copper oxide or copper carbonate and potassium fluoride or potassium bifluoride into hydrofluoric acid, and magnetically stirring to obtain a precipitate;
(3) washing the precipitate with ethanol, and drying to obtain the perovskite fluoride luminescent material.
4. The method for preparing perovskite fluoride luminescent material as claimed in claim 3, wherein in the step (2), the temperature of the magnetic stirring is 18-25 ℃, the speed is 400-600r/min, and the time is 10-15 h.
5. The method for producing a perovskite fluoride luminescent material according to claim 3, wherein in the step (3), the number of washing with ethanol is 4 to 6.
6. The method for preparing a perovskite fluoride luminescent material according to claim 3, wherein in the step (3), the drying temperature is 60-90 ℃ and the drying time is 24-48 h.
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