CN115612495B - Silicate fluorescent powder with high brightness and high stability and preparation method thereof - Google Patents
Silicate fluorescent powder with high brightness and high stability and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- 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
- C09K11/77742—Silicates
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21K—NON-ELECTRIC LIGHT SOURCES USING LUMINESCENCE; LIGHT SOURCES USING ELECTROCHEMILUMINESCENCE; LIGHT SOURCES USING CHARGES OF COMBUSTIBLE MATERIAL; LIGHT SOURCES USING SEMICONDUCTOR DEVICES AS LIGHT-GENERATING ELEMENTS; LIGHT SOURCES NOT OTHERWISE PROVIDED FOR
- F21K9/00—Light sources using semiconductor devices as light-generating elements, e.g. using light-emitting diodes [LED] or lasers
- F21K9/60—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction
- F21K9/64—Optical arrangements integrated in the light source, e.g. for improving the colour rendering index or the light extraction using wavelength conversion means distinct or spaced from the light-generating element, e.g. a remote phosphor layer
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
- F21Y2115/00—Light-generating elements of semiconductor light sources
- F21Y2115/10—Light-emitting diodes [LED]
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Abstract
The invention belongs to the field of inorganic luminescent materials, and particularly relates to a high-brightness high-stability narrow-band green light emission fluorescent powder and a preparation method thereof. The chemical formula is: naLa (NaLa) 1‑x‑y SiO 4 :xTb 3+ ,yCe 3+ Wherein 0 is<x is more than or equal to 0.22,0 and y is more than or equal to 0.22. The invention selects NaLaSiO 4 The matrix belongs to an orthogonal structure of a Pnma space group and has excellent stability. With Tb 3+ Is a luminescence center, passes through Ce 3+ →Tb 3+ The energy transfer of the fluorescent powder is synthesized into the high-efficiency narrow-band green light emitting fluorescent powder. The high-temperature carbothermic reduction method has the advantages of simple process, low cost, high yield and the like, and can meet the requirement of industrial mass production. The fluorescent powder prepared by the invention has good application potential in the field of backlight source display and LED illumination.
Description
Technical Field
The invention relates to a high-brightness high-stability narrow-band green light emission fluorescent powder and a preparation method thereof, belonging to the technical field of inorganic luminescent materials.
Background
As a new generation of illumination sources, white Light Emitting Diodes (LEDs) have a very broad application prospect, and the fields mainly included at present are illumination and Liquid Crystal Display (LCD) backlight display. In the field of photographs, compared with traditional illumination sources such as incandescent lamps, fluorescent lamps and the like, the white light LED has the obvious advantages of high luminous efficiency, energy conservation, environmental protection, long service life and the like. But low Color Rendering Index (CRI) and high color temperature (CCT) still prevent their further development. In the display field, compared with the traditional Cold Cathode Fluorescent Lamp (CCFL), the LED has the advantages of small volume, low power consumption, long service life, no mercury and the like as a backlight source of the LCD. Although LCDs currently occupy the major market in the display field, performance of color gamut and the like of LCDs needs to be further improved compared to emerging displays such as organic light emitting diode displays (OLEDs), quantum dot light emitting diode displays (QLEDs) and the like, so as to meet the social requirement for image display quality. LEDs as LCD backlights have a significant impact on the performance of LCD color gamut, etc., which is mainly reflected in the full width at half maximum (FWHM), lifetime, thermal stability, etc. of the constituent LED phosphors. Therefore, searching for a high-efficiency fluorescent powder with small half-peak width, good stability and short service life, which can improve the color rendering index of an LED and reduce the color temperature, becomes a urgent concern for researchers.
In recent years, orthosilicate phosphors have received extensive attention from researchers due to their simple structure and good physicochemical properties. Compared with other salt fluorescent powder, the preparation cost is lower and the synthesis is easy. Some rare earth doped silicate luminescent materials have been reported in the prior art, for example, patent CN112480910a reports a Ba a Ca b SiO 4 :xEu 2+ ,yR 3+ (r=er, nd, lu, yb, gd, ho, dy) phosphor, which has afterglow effect and FWHM close to 100nm, although it has good thermal stability; patent CN114316956a was synthesized (Sr, ba) using liquid phase method 2 SiO 4 :0.03Eu 2+ The fluorescent powder has the advantages that the thermal preparation method of the fluorescent powder is complex, the time is long, the reducing atmosphere is required to be introduced, and the large-scale production is not facilitated; patent CN114316979A synthesized M by high temperature solid phase method 4-x N 6 O(SiO 4 ) 6 :xEu 2+ (m=ca, sr, ba; n=y, la, gd, lu) green phosphor, but its FWHM is large and is not suitable for display field. From these reports, it can be seen that it is difficult to find a composition satisfying high thermal stabilityA light emitting material with various requirements such as small FWHM and short lifetime. The invention adopts the NaLaSiO synthesized by the high-temperature solid phase method 4 :Tb 3+ ,Ce 3+ The fluorescent powder is convenient to produce and easy to obtain. And has the advantages of high thermal stability, small half-peak width, short service life and the like. The requirements of the backlight source display and LED illumination fields can be better met.
The invention successfully prepares the fluorescent powder for emitting narrow-band green light with high brightness and high stability through a simple high-temperature carbothermic reduction process for the first time. The silicate is selected as a matrix material, so that the fluorescent powder has excellent thermal stability; with Tb 3+ Replacement of La in matrix 3+ Ions, on the basis of ensuring charge balance, obtaining a luminescent material with green light emission and small FWHM; in addition, ce 3+ Ion introduction, tb is further improved by energy transfer 3+ Enables the material to obtain a better color gamut.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a rare earth doped NaLaSiO with simple structure, high brightness and high stability 4 Luminescent materials.
The technical scheme of the invention is as follows: the chemical formula of the luminescent material is as follows: naLa (NaLa) 1-x-y SiO 4 :xTb 3+ ,yCe 3+ Wherein 0 is<x is more than or equal to 0.22,0 and y is more than or equal to 0.22. The fluorescent powder has absorption in the range of 250-380 nm. After experimental preference, the optimal doping ratio of the fluorescent powder is x=0.18 and y=0.06.
The second technical problem to be solved by the invention is to provide a preparation method of high-brightness high-stability narrow-band green light emission fluorescent powder.
A preparation method of high-brightness high-stability narrow-band green light emission fluorescent powder comprises the following specific steps:
a. according to NaLa 1-x-y SiO 4 :xTb 3+ ,yCe 3+ (0<x is more than or equal to 0.22,0 and y is more than or equal to 0.22), and anhydrous sodium carbonate (Na) is weighed 2 CO 3 ) Lanthanum oxide (La) 2 O 3 ) Silicon dioxide (SiO) 2 ) Terbium oxide (Tb) 4 O 7 ) Cerium oxide (CeO) 2 ) And activated carbon powder, putting the activated carbon powder into an agate mortar for grinding until the activated carbon powder is uniform;
b. transferring the mixed powder obtained by grinding in the step a into a corundum crucible, placing the corundum crucible into a tube furnace, and adding N into the corundum crucible 2 And (5) heating and calcining under the protective atmosphere, and cooling to obtain a white solid product.
In one embodiment, in step a, the anhydrous sodium carbonate is in excess of 5 to 10%; preferably, the anhydrous sodium carbonate is in an excess of 10%.
In one embodiment, in step a, the amount of activated carbon powder is 2 to 6wt%; preferably, the amount of activated carbon powder is 4wt%.
In one embodiment, in step a, the milling time is from 10 to 30 minutes; preferably, the milling time is 20 minutes.
In one embodiment, in step b, N 2 The flow rate of the water is controlled to be 20-50 ml/min; preferably, N 2 The flow rate of (C) was controlled at 30ml/min.
In one embodiment, in step b, the tube furnace calcination temperature is 800 to 1100 ℃; preferably, the tube furnace calcination temperature is 1100 ℃.
In one embodiment, in the step b, the calcination heat preservation time of the tube furnace is 3-4 hours; preferably, the calcination heat preservation time of the tube furnace is 3 hours.
The third technical problem to be solved by the invention is to provide the application of the high-brightness high-stability narrow-band green light emission fluorescent powder, which is applied to the fields of backlight source display and LED illumination.
The invention has the beneficial effects that:
1. the invention creatively uses NaLaSiO 4 The matrix is used as a matrix for the phosphor and is synthesized by a high temperature solid phase method. The matrix has simple structure and stable physical and chemical properties; the method is simple and quick;
2. the invention is creatively disclosed in NaLaSiO 4 Rare earth luminescent ion Tb doped in matrix 3+ And introducing Ce on the basis 3+ Ion, through Tb 3+ →Ce 3+ The energy transfer of the fluorescent powder is further improved;
3. the product of the invention has the characteristics of no toxicity, no pollution, excellent physical and chemical properties and the like. And the white light with high color rendering index and low color temperature can be obtained after the white light is combined with near ultraviolet chips and commercial red and blue fluorescent powder. And the smaller half-peak width can well improve the color gamut of the LCD when the LCD is used as a backlight source.
Drawings
FIG. 1 shows the NaLa obtained in examples 1 and 2 0.82 SiO 4 :0.18Tb 3+ And NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ XRD pattern of phosphor.
FIG. 2 shows the NaLa obtained in example 1 0.82 SiO 4 :0.18Tb 3+ Fluorescence spectrum of the phosphor.
FIG. 3 shows NaLa obtained in example 2 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Fluorescence spectrum of phosphor (containing NaLa 0.82 SiO 4 :0.18Tb 3+ Emission spectrum of phosphor).
FIG. 4 shows the optimal sample NaLa obtained in examples 1 and 2 0.82 SiO 4 :0.18Tb 3+ And NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Is not shown.
FIG. 5 shows NaLa obtained in example 2 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Fluorescent lifetime graph of (2).
FIG. 6 shows the reaction product of example 2 with NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ And combining commercial blue and red fluorescent powder with an ultraviolet chip to obtain the w-LED graph.
FIG. 7 shows the optimal sample NaLa obtained in examples 1 and 2 0.82 SiO 4 :0.18Tb 3+ And NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ CIE color coordinate diagram of (a).
Detailed Description
The invention has been tested several times in succession, and the invention will now be described in further detail with reference to a few test results, which are described in detail below in connection with specific examples.
Example 1
NaLa 0.82 SiO 4 :0.18Tb 3+ The synthesis process comprises the following steps:
1) According to NaLa 0.82 SiO 4 :0.18Tb 3+ Stoichiometric ratio anhydrous sodium carbonate (Na) 2 CO 3 ) 0.3498g (10% excess), lanthanum oxide (La) 2 O 3 ) 0.8406g, silicon dioxide (SiO) 2 ) 0.3605g, terbium oxide (Tb) 4 O 7 ) 0.2019g and 0.0701g of activated carbon powder are put into an agate mortar for grinding for 20min until uniform.
2) Transferring the mixed powder obtained in the step 1) into a corundum crucible and placing the corundum crucible into a tube furnace, and adding N with the flow rate of 30ml/min 2 Calcining for 3h at 1100 ℃ under the protection atmosphere, and cooling to obtain a white solid product.
FIG. 1 contains NaLa 0.82 SiO 4 :0.18Tb 3+ XRD patterns of fluorescent powder, from which the sample and NaLaSiO can be seen 4 The standard diffraction peaks of (2) match well, confirming successful synthesis of the sample.
FIG. 2 shows the measurement of NaLa using a fluorescence spectrophotometer (Hitachi F-4600, japan) 0.82 SiO 4 :0.18Tb 3+ Fluorescence spectrum of the phosphor. As can be seen from the figure, tb 3+ The ion is a luminescence center, and under the excitation of the ultraviolet wavelength of 377nm, the fluorescent powder presents the strongest emission peak at 544nm, and emits bright green light.
Example 2
NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ The synthesis process comprises the following steps:
1) According to NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Stoichiometric ratio anhydrous sodium carbonate (Na) 2 CO 3 ) 0.3498g (10% excess), lanthanum oxide (La) 2 O 3 ) 0.7429g, silicon dioxide (SiO) 2 ) 0.3605g, terbium oxide (Tb) 4 O 7 ) 0.2019g, cerium oxide (CeO) 2 ) 0.1033g and 0.0703g of activated carbon powder are put into an agate mortar for grinding for 20min until uniform.
2) Transferring the mixed powder obtained in the step 1) into a corundum crucible and placing the corundum crucible into a tube furnace, and adding N with the flow rate of 30ml/min 2 Under the protection atmosphere, underCalcining at 1100 ℃ for 3 hours, and cooling to obtain a white solid product.
FIG. 1 contains NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ XRD patterns of fluorescent powder, from which the sample and NaLaSiO can be seen 4 The standard diffraction peak of (2) is well matched, and a proper amount of Ce is proved 3+ The original structure of the fluorescent powder is not damaged by the introduction, and the target product is successfully synthesized.
FIG. 3 shows the measurement of NaLa using a fluorescence spectrophotometer (Hitachi F-4600, japan) 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Fluorescence spectrum of the phosphor. As can be seen from fig. 3, at Tb 3+ Ce is introduced based on the ion as the luminescence center 3+ After ions, the ultraviolet absorption intensity of the fluorescence peak is obviously improved. The strongest excitation peak is at 346nm and its emission intensity is higher than that of the emission without Ce 3+ The ion front is improved by nearly 8 times. In addition, the FWHM is only 13.24nm, which is far smaller than other common fluorescent powder.
FIG. 4 shows NaLa 0.82 SiO 4 :0.18Tb 3+ ，NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ Thermal stability profile of the sample. As can be seen from the graph, at the typical operating temperature of 150 ℃, the luminescence performance of both samples can be maintained at more than 90% at room temperature, which is higher than that of the typical commercial phosphors.
The fluorescence lifetime graph of fig. 5 shows: naLa (NaLa) 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ The phosphor lifetime is only 2.521ms. The short lifetime can reduce the occurrence of "ghosts" in the display, thus facilitating the use of the phosphor in backlight displays.
FIG. 6 is NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ And (5) a packaged w-LED graph. From the figure, it can be seen that the chip has a good color rendering index (ra=85.1) and a low correlated color temperature (cct=4359), shows bright warm white light, and shows potential value in the field of LED illumination.
FIG. 7 is NaLa 0.82 SiO 4 :0.18Tb 3+ And NaLa 0.76 SiO 4 :0.18Tb 3+ ,0.06Ce 3+ And a CIE color coordinate graph after the two are packaged. As can be seen from the figure, ce 3+ The introduction of the hetero ions improves the color purity of the fluorescent powder, so that the fluorescent powder is more biased to the green light part, and can reach 77.24% of the standard NSTC color gamut. And also tends to warm white areas after encapsulation.
Claims (9)
1. A high-brightness high-stability narrow-band green light emitting fluorescent powder is characterized in that: the chemical formula of the fluorescent powder is NaLa 1-x- y SiO 4 :xTb 3+ ,yCe 3+ Wherein 0 is<x≤0.22，0≤y≤0.22。
2. NaLa according to claim 1 1-x-y SiO 4 :xTb 3+ ,yCe 3+ The preparation method of the fluorescent powder is characterized by comprising the following specific steps of:
a. according to NaLa 1-x-y SiO 4 :xTb 3+ ,yCe 3+ (0<x is more than or equal to 0.22,0 and y is more than or equal to 0.22), anhydrous sodium carbonate, lanthanum oxide, silicon dioxide, terbium oxide, cerium oxide and active carbon powder are weighed and put into an agate mortar for grinding until uniformity;
b. transferring the mixed powder obtained by grinding in the step a into a corundum crucible, placing the corundum crucible into a tube furnace, and adding N into the corundum crucible 2 And (5) heating and calcining under the protective atmosphere, and cooling to obtain a white solid product.
3. The method for preparing the high-brightness high-stability narrow-band green light emitting fluorescent powder according to claim 2, which is characterized in that: in the step a, the excess of anhydrous sodium carbonate is 5-10%.
4. The method for preparing the high-brightness high-stability narrow-band green light emitting fluorescent powder according to claim 2, which is characterized in that: in the step a, the using amount of the activated carbon powder is 2-6wt%.
5. The method for preparing the high-brightness high-stability narrow-band green light emitting fluorescent powder according to claim 2, which is characterized in that: in the step a, the grinding time is 10-30 min.
6. The method for preparing the high-brightness high-stability narrow-band green light emitting fluorescent powder according to claim 2, which is characterized in that: in step b, N 2 The flow rate of the water is controlled to be 20-50 ml/min.
7. The method for preparing high-brightness high-stability narrow-band green light-emitting phosphor according to claim 2, wherein in step b, the tube furnace calcination temperature is 800-1100 ℃.
8. The method for preparing the high-brightness high-stability narrow-band green light emitting fluorescent powder according to claim 2, wherein in the step b, the calcination heat preservation time of the tube furnace is 3-4 hours.
9. The use of a high-luminance high-stability narrow-band green-emitting phosphor according to claim 1 or a high-luminance high-stability narrow-band green-emitting phosphor produced by the production method according to any one of claims 2 to 8, characterized in that the phosphor is used in the fields of backlight display and LED illumination.
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