CN114989824A - Short life spheroidal Mn 4+ Fluoride-doped red fluorescent powder, structure, preparation method and light-emitting device - Google Patents
Short life spheroidal Mn 4+ Fluoride-doped red fluorescent powder, structure, preparation method and light-emitting device Download PDFInfo
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- 229910001506 inorganic fluoride Inorganic materials 0.000 claims abstract description 4
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- 229910052751 metal Inorganic materials 0.000 claims description 6
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Abstract
The invention relates to the technical field of luminescent materials, in particular to short-life sphere-like Mn 4+ The fluoride-doped red fluorescent powder, the structure, the preparation method and the light-emitting device can be effectively excited by blue light to emit narrow-band red light, have short fluorescent life and excellent tolerance, are suitable for the field of ultra-wide color gamut miniLEDs for backlight display, and are characterized in that: it comprises an inorganic fluoride comprising M 1 、M 2 、M 3 F, and Mn at the luminescence center 4+ The chemical formula of which can be expressed as M 1 3 M 2 3 M 3 a F 12 :xMn 4 (ii) a Wherein M is 1 Is Li element, M 2 The element is selected from Na, K, Ru and NH 4+ At least one of alkali metal ions; m 3 Is trivalent metal ion such as Al, Ga, Sc, etcThe fluorescent powder structure of at least one of the above-mentioned materials is in the form of spheroidal polyhedron, and its preparation method includes the steps of mixing raw materials, stirring, standing still, filtering, washing and drying; a light source of a light emitting device and the phosphor prepared by the method.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to short-life sphere-like Mn 4+ Doped fluoride red fluorescent powder, a structure, a preparation method and a light-emitting device.
Background
Since the 20 th century and 70 s break through high-brightness blue Light Emitting Diodes (LEDs), white LEDs have the advantages of low voltage, high lighting effect, low energy consumption, long life, no pollution, small size, fast response, low heat generation, high reliability and the like, and thus, they have rapidly become the mainstream of green solid-state lighting in the fourth generation. At present, white light LEDs are widely applied to the fields of illumination in various places, backlight display and the like. At present, the white light LED used in backlight display is mainly formed by combining a blue light LED chip and green and red fluorescent powder materials. Since the display field has high requirements for color purity, color gamut, reaction time, and the like, the phosphor is required to have the characteristics of high luminous efficiency, narrow half-wave width, good thermal stability, and the like. The red phosphor material is a key material for determining the color gamut of the backlight module. At present, red phosphor materials which have been commercialized include nitride red powder and fluoride red powder. The nitride red fluorescent powder gradually exits from the market of the display field because the nitride red fluorescent powder has larger half-wave width of an emission peak and low color purity, and cannot meet the requirement of wide color gamut.
Mn 4+ The fluoride-doped fluorescent powder material has a strong absorption band in a near ultraviolet-blue light region, and emits narrow-band red light under the excitation of blue light, thereby attracting wide attention of people. There are many Mn 4+ Doped fluoride phosphor materials have been reported.Wherein A is 2 MF 6 :Mn 4+ The method has the advantages of high internal and external quantum efficiency, excellent thermal quenching stability and the like, and is widely applied to the display fields of various application occasions such as mobile phones, televisions and the like. However, A 2 MF 6 :Mn 4+ Has the defects of poor moisture resistance, insufficient appearance uniformity, long fluorescent afterglow and the like in the packaging process. With the continuous market promotion of miniLED technology, the defects are more and more prominent, and the requirements of ultra-wide color gamut, quick response and the like cannot be met. In order to overcome these disadvantages, the present invention aims to develop a fluoride phosphor having a spherical shape, a short fluorescent life, and excellent moisture resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, adapt to practical requirements and provide the short-life spheroidal Mn 4+ The fluoride-doped red fluorescent powder, the structure, the preparation method and the light-emitting device can be effectively excited by blue light to emit narrow-band red light, have short fluorescent life and excellent tolerance, and are suitable for the field of ultra-wide color gamut miniLEDs for backlight display.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
the invention discloses a short-life spheroidal Mn 4+ Doped fluoride red phosphor comprising an inorganic fluoride including M 1 、M 2 、M 3 F, and Mn at the luminescence center 4+ The chemical formula of which can be expressed as M 1 3 M 2 3 M 3 a F 12 :xMn 4 (ii) a Wherein M is 1 Is Li element, M 2 The element is selected from Na, K, Ru and NH 4+ At least one of alkali metal ions; m 3 Is at least one of trivalent metal ions such as Al, Ga, Sc and the like, and necessarily contains Sc element; wherein, 1 is more than or equal to a<2，0<x≤1。
The M is 1 Preferably Li element or M 1 Is Na.
Said M 2 Preferably Na element, M 3 Is Sc.
The short-lived quasi-spherical Mn 4+ The fluorescence lifetime of the red fluorescent powder doped with fluoride does not exceed 2 us.
Furthermore, the invention also discloses a short-life spheroidal Mn 4+ Fluoride-doped red phosphor structure, this short-lived quasi-spherical Mn 4+ The fluoride-doped red phosphor structure exhibits a spheroidal polyhedron shape and is comprised of a short-lived spheroidal Mn as described above 4+ Doped with fluoride red fluorescent powder.
The short-lived quasi-spherical Mn 4+ The particle size of the red doped fluoride fluorescent powder structure is 100-1000 nm.
Furthermore, the invention also discloses a short-life spheroidal Mn 4+ The preparation method of the red fluorescent powder doped with fluoride comprises the following steps:
s1, taking 100ml of 40% HF solution as a solvent, and adding 10-20g of KMnO 4 And 5-10g KHF 2 The mixture reacts to prepare a precursor K 2 MnF 6 By settling or centrifuging 2 MnF 6 A solid;
s2, taking 50ml of 40 percent HF solution as a solvent, and weighing the solution containing 0.001-0.005mol of metal element M 3 Continuously stirring the corresponding simple substance or compound to fully react;
s3, after the product obtained in the step S2 is completely dissolved, respectively adding M containing 0.0015-0.0075mol of metal element 1 、M 2 And the precursor K prepared in the first step 2 MnF 6 ；
S4, continuously stirring and reacting for 20-60min to fully react;
s5, standing and precipitating for 1-3h, or centrifuging at the speed of 1000-6000r/min to quickly separate out solids;
s6, filtering;
s7, washing for 4-5 times by using ethanol or acetone;
s8, drying at 40-80 ℃ to obtain the product.
Further, the present invention also discloses a light emitting device, comprising a light source and a phosphor, characterized in that: the fluorescent powder is prepared by the method.
The invention has the beneficial effects that:
the fluorescent powder related by the invention is in a sphere-like shape, has the characteristics of regular height, uniformity and small particle size, has short fluorescent service life, and has good applicability in the field of MiniLED.
Drawings
FIG. 1 shows the composition Li in example 5 3 Na 3 Sc 2 F 12 :0.01Mn 4+ The excitation and emission spectra of the phosphor.
FIG. 2 shows the composition Li in example 6 3 Na 3 (Sc 0.8 Al 0.2 ) 2 F 12 :0.01Mn 4+ SEM image of the phosphor of (1).
Detailed Description
The invention is further illustrated with reference to the following figures and examples:
example 1: short-life spheroidal Mn 4+ Doped with fluoride red phosphor.
It comprises an inorganic fluoride comprising M 1 、M 2 、M 3 F, and Mn at the luminescence center 4+ The chemical formula of which can be expressed as M 1 3 M 2 3 M 3 a F 12 :xMn 4+ (ii) a Wherein M is 1 Is Li element, M 2 The element is selected from Na, K, Ru and NH 4+ At least one of alkali metal ions; m is a group of 3 Is at least one of trivalent metal ions such as Al, Ga, Sc and the like, and necessarily contains Sc element; wherein, 1 is more than or equal to a<2，0<x≤1。
In this embodiment, M 1 Preferably Li element or M 1 Is Na.
In this embodiment, M 2 Preferably Na element, M 3 Is Sc.
In this example, the short-lived quasi-spherical Mn 4+ The fluorescence lifetime of the red fluorescent powder doped with fluoride does not exceed 2 us.
Example 2A short-lived spheroidal Mn 4+ Doped fluoride red phosphor structure.
This short lifeSpheroidal Mn 4+ The doped fluoride red phosphor structure exhibits a spheroidal shape and is comprised of a short-lived spheroidal Mn as described in example 1 4+ The red fluorescent powder doped with fluoride is prepared, and the particle size is 100-1000 nm.
Example 3A short lived spheroidal Mn 4+ Preparation of fluoride-doped Red phosphor for short-lived spheroidal Mn as described in example 2 4+ The fluoride-doped red fluorescent powder structure comprises the following steps:
s1, taking 100ml of 40% HF solution as a solvent, and adding 10-20g of KMnO 4 And 5-10g KHF 2 The mixture reacts to prepare a precursor K 2 MnF 6 By settling or centrifuging 2 MnF 6 A solid;
s2, taking 50ml of 40 percent HF solution as a solvent, and weighing the solution containing 0.001-0.005mol of metal element M 3 Continuously stirring the corresponding simple substance or compound to fully react;
s3, respectively adding 0.0015-0.0075mol of metal element M after the product obtained in the step S2 is completely dissolved 1 、M 2 And the precursor K prepared in the first step 2 MnF 6 ；
S4, continuously stirring and reacting for 20-60min to fully react;
s5, standing and precipitating for 1-3 h;
s6, filtering;
s7, washing for 4-5 times by using ethanol or acetone;
s8, drying at 40-80 ℃ to obtain the product.
Embodiment 4 also discloses a light-emitting device comprising a light source and a phosphor prepared by the method of embodiment 3.
Example 5, one of the specific application examples of the present invention is as follows:
according to the chemical formula Li of the phosphor 3 Na 3 Sc 2 F 12 :0.01Mn 4+ 。
Firstly weighing 0.2758gSc 2 O 3 Adding into 40% HF solution, and stirring for 30minUntil the solution is clear.
0.0395gK is then weighed 2 MnF 6 Adding into the obtained solution, and stirring for 20min to K 2 MnF 6 Complete dissolution gave an orange solution.
0.2217gLiF, 0.3180gNaF were weighed out, mixed well in a mortar, and the mixture was quickly added to the orange solution obtained above and stirring was continued for 60min until a large amount of orange precipitate appeared.
Centrifugation was carried out using a centrifuge to obtain an orange powder.
The orange powder was washed with ethanol solution 2-3 times, placed in an oven and dried at 60 ℃.
The fluorescent powder prepared by the embodiment is subjected to a luminescence property test, an excitation spectrum (625nm monitoring) and an emission spectrum (475nm excitation) of the fluorescent powder are shown in the attached figure 1, and it can be seen that the excitation wavelength range covers 260-450 nm, the emission wavelength covers 410-575 nm, the peak wavelength is 474nm, and the fluorescence lifetime is 1.98 us.
Example 6, another example of a specific application of the present invention is as follows:
according to the chemical formula Li of the phosphor 3 Na 3 (Sc 0.8 Al 0.2 ) 2 F 12 :0.01Mn 4+ 。
Firstly weighing 0.2206gSc 2 O 3 ，0.033gAl 2 O 3 It was added to a 40% HF solution and stirred for 30min until the solution was a clear solution.
0.0395gK is then weighed 2 MnF 6 Adding into the obtained solution, and stirring for 20min to K 2 MnF 6 Complete dissolution gave an orange solution.
0.1438g of LiOH and 0.24g of NaOH were weighed out, mixed well in a mortar, and the mixture was quickly added to the orange solution obtained above and stirring was continued for 60min until a large amount of orange precipitate appeared.
Centrifugation was carried out using a centrifuge to obtain an orange powder.
The orange powder was washed with acetone solution 2-3 times and then placed in an oven and dried at 50 ℃.
The morphology of the phosphor powder prepared in this example was observed to be spheroidal polyhedral by SEM (as shown in FIG. 2). The test of the luminous property shows that: the excitation wavelength range covers 260-450 nm, the emission wavelength covers 410-575 nm, the peak wavelength is 474nm, and the fluorescence lifetime is 1.8 us.
The embodiments of the present invention are disclosed as the preferred embodiments, but not limited thereto, and those skilled in the art can easily understand the spirit of the present invention and make various extensions and changes without departing from the spirit of the present invention.
Claims (10)
1. Short-life spheroidal Mn 4+ Doping fluoride red fluorescent powder; the method is characterized in that: it comprises an inorganic fluoride comprising M 1 、M 2 、M 3 F, and Mn in the luminescence center 4+ The chemical formula of which can be expressed as M 1 3 M 2 3 M 3 a F 12 :xMn 4 (ii) a Wherein M is 1 Is Li element, M 2 The element is selected from Na, K, Ru and NH 4+ At least one of alkali metal ions; m 3 Is at least one of trivalent metal ions such as Al, Ga, Sc and the like, and necessarily contains Sc element; wherein, 1 is less than or equal to a<2，0<x≤1。
2. The short-lived spheroidal Mn of claim 1 4+ The fluoride-doped red fluorescent powder is characterized in that: m 1 Is Li element or M 1 Is Na.
3. The short-lived spheroidal Mn of claim 1 4+ The fluoride-doped red fluorescent powder is characterized in that: m 2 Is Na element, M 3 Is Sc.
4. Short-life spheroidal Mn 4+ A fluoride-doped red phosphor structure; the method is characterized in that: the short life spheroidal Mn 4+ Doped fluoride RedThe colored phosphor structure exhibits a spheroidal polyhedron shape and is represented by the short-lived spheroidal Mn of any one of claims 1 to 3 4+ Doped with fluoride red fluorescent powder.
5. The short-lived spheroidal Mn of claim 1 4+ The fluoride-doped red fluorescent powder structure is characterized in that: the short-lived quasi-spherical Mn 4+ The particle size of the red doped fluoride fluorescent powder structure is 100-1000 nm.
6. Short-life spheroidal Mn 4+ The preparation method of the fluoride-doped red fluorescent powder is characterized by comprising the following steps of:
s1, taking 100ml of 40% HF solution as a solvent, and adding 10-20g of KMnO into the solvent 4 And 5-10g KHF 2 The mixture reacts to prepare a precursor K 2 MnF 6 By settling or centrifuging 2 MnF 6 A solid;
s2, taking 50ml of 40 percent HF solution as a solvent, and weighing the solution containing 0.001-0.005mol of metal element M 3 Continuously stirring the corresponding simple substance or compound to fully react;
s3, respectively adding 0.0015-0.0075mol of metal element M after the product obtained in the step S2 is completely dissolved 1 、M 2 And the precursor K prepared in the first step 2 MnF 6 ；
S4, continuously stirring to enable the mixture to fully react;
s5, standing for precipitation or centrifuging to separate out solids;
s6, filtering;
s7, washing;
and S8, drying to obtain the product.
7. The short-lived spheroidal Mn of claim 1 4+ The preparation method of the fluoride-doped red fluorescent powder is characterized by comprising the following steps:
in step S4, stirring and reacting for 20-60 min;
in the step S5, standing and precipitating for 1-3h, or centrifuging at the speed of 1000-6000 r/min;
in step S7, wash with ethanol or acetone 4-5 times.
In step S8, drying at 40-80 deg.C.
8. The short-lived spheroidal Mn of claim 1 4+ The preparation method of the fluoride-doped red fluorescent powder is characterized by comprising the following steps: in step S2, M 3 The corresponding compounds include fluorides, hydroxides, oxides, carbonates or nitrates.
9. The short-lived spheroidal Mn of claim 1 4+ The preparation method of the fluoride-doped red fluorescent powder is characterized by comprising the following steps: in step S3, M 1 、M 2 The corresponding compounds include fluorides, hydroxides, oxides, carbonates or nitrates.
10. A light-emitting device comprises a light source and fluorescent powder, and is characterized in that: the phosphor is formed of the short-lived spheroidal Mn of any one of claims 6 to 9 4+ The preparation method of the red fluorescent powder doped with fluoride.
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|---|---|---|---|---|
| CN117165287A (en) * | 2023-06-16 | 2023-12-05 | 江苏博睿光电股份有限公司 | Red narrow-band fluorescent powder and preparation method and application thereof |
| CN117165287B (en) * | 2023-06-16 | 2024-05-14 | 江苏博睿光电股份有限公司 | Red narrow-band fluorescent powder and preparation method and application thereof |
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