CN113372915B - Single-phase fluorescent material for white light LED and preparation method and application thereof - Google Patents
Single-phase fluorescent material for white light LED and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 239000006104 solid solution Substances 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical group [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 8
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 23
- 239000002244 precipitate Substances 0.000 description 15
- 229910001220 stainless steel Inorganic materials 0.000 description 15
- 239000010935 stainless steel Substances 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 239000003814 drug Substances 0.000 description 10
- 230000005284 excitation Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000295 emission spectrum Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 229940079593 drug Drugs 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000004809 Teflon Substances 0.000 description 5
- 229920006362 Teflon® Polymers 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009877 rendering Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
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- H01L33/50—Wavelength conversion elements
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Abstract
The invention discloses a single-phase fluorescent material for a white light LED (light-emitting diode) and a preparation method and application thereof 2 Sn 1‑x‑y Te x Bi y Cl 6 And x has a value range of 0<x<1, y is not less than 0.05 and not more than 0.22; and mixing the Cs source, the Sn source, the Te source, the Bi source and hydrochloric acid according to a set molar ratio, and carrying out hydrothermal reaction to obtain the single-phase fluorescent material for the white light LED. The invention mixes the raw material components with hydrochloric acid, then the raw material components are dissolved and reacted under the action of high temperature and high pressure in the hydrothermal process, and then the mixture is separated out in a new crystal structure, so that the single-phase solid solution material is obtained and is used for manufacturing a light-emitting device.
Description
Technical Field
The invention belongs to the technical field of inorganic luminescent materials, and relates to a single-phase fluorescent material for a white light LED, and a preparation method and application thereof.
Background
Light Emitting Diodes (LEDs) have a series of excellent properties such as high photoelectric conversion efficiency, environmental friendliness, long service life, fast response, and the like, and thus are considered as new light sources in the next generation of illumination and display fields. The principle is that excited electrons in semiconductors jump from an excited state back to the ground state release energy in the form of photons, thereby emitting light of different wavelengths.
The currently mainstream white light emitting diode (wLED) utilizes the principle of three primary colors to excite fluorescent powder of complementary color (yellow) by a blue light chip, and finally, white light is obtained by mixing. For example, the manufacturing method of the YAG phosphor disclosed in CN101838536A and the preparation method of the silicate yellow phosphor disclosed in CN106118635A both use a blue LED chip as a base and mix with a fluorescent material emitting yellow light to obtain white light, but the blue light in such a white light emitting diode (wLED) is not only used as a white light synthesized light source, but also used as an excitation light source of yellow light, and the problem of color temperature change due to mismatch between blue light and yellow light inevitably occurs under the condition of current change. In addition, the half-height width of the two combined lights in the white light emitting diode (wLED) is not ideal in coverage of the whole visible light range, so that the color rendering index is lower than the indoor lighting requirement, although corresponding improvement measures are taken, for example, the full-spectrum LED phosphor composition disclosed in CN112608750A and the full-spectrum white light LED device adopt a method of increasing the red fluorescent component to increase the color rendering index of the device. However, this method can raise the color rendering index and also bring about the problem of color shift caused by the difference in decay rate and lifetime between fluorescent materials. In addition, the thermal stability of the fluorescent material, the complexity of the process, etc. are also issues to be considered in the material design and device manufacturing process.
Disclosure of Invention
Aiming at the problems of the existing fluorescent material for the white light LED, the invention aims to provide a single-phase fluorescent material for the white light LED which can be excited by ultraviolet, a preparation method and application thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a single-phase fluorescent material for white LED is prepared from single-phase solid solution with molecular formula of Cs 2 Sn 1-x- y Te x Bi y Cl 6 And x has a value range of 0<x<1, y is more than or equal to 0.05 and less than or equal to 0.22.
The invention also provides a preparation method of the single-phase fluorescent material for the white light LED, which comprises the steps of mixing the Cs source, the Sn source, the Te source, the Bi source and hydrochloric acid according to a set molar ratio, and carrying out hydrothermal reaction to obtain the single-phase fluorescent material for the white light LED.
Preferably, the Cs source is CsCl; the Sn source is SnCl 2 、SnCl2·2H 2 O or SnCl 4 (ii) a The Te source is TeO 2 Or TeCl 4 (ii) a The source of Bi is Bi 2 O 3 Or BiCl 3 。
Preferably, the hydrochloric acid is concentrated hydrochloric acid with the mass fraction of 36-38%.
Preferably, the temperature of the hydrothermal reaction is 150-200 ℃; the time is 5-18 h.
Preferably, the temperature reduction rate after the hydrothermal reaction is not higher than 5 ℃/h.
The invention also provides application of the single-phase fluorescent material for the white light LED, and the single-phase fluorescent material is used for manufacturing a luminescent device.
In the invention, the raw material components are mixed with hydrochloric acid, dissolved and reacted under the action of high temperature and high pressure in the hydrothermal process, and then separated out in a new crystal structure, thereby obtaining the single-phase solid solution material. Wherein Te atom and Bi atom pair Cs 2 SnCl 6 The substitution of Sn atoms in the crystal lattice of the perovskite material introduces new impurity energy bands in the original band gap, and the transition of the new impurity energy bands to the valence band brings blue and yellow visible light emission respectively, and finally white light is obtained by mixing. Meanwhile, Jahn-Teller distortion occurs to an octahedron in the perovskite due to atomic solid solution, the formation of a self-trapping exciton state is aggravated, and an emission peak is widened when a radiation transition from the self-trapping exciton state to a ground state occurs, so that the fluorescence of the material has a higher color rendering index.
Compared with the prior art, the invention has the following advantages:
1. the invention is a solid solution, the fluorescence luminescence can be adjusted and controlled along with the change of the solid solubility of the components, and the color temperature can be adjusted and controlled from cold white light to warm white light.
2. The invention is a single-phase fluorescent material, and avoids the problems of color drift and the like caused by different attenuation rates and service lives of various fluorescent materials when a white light LED is built.
3. The broadening of the emission peak caused by the radiative transition that occurs from the trapped exciton state also makes the material inherently possess a higher color rendering index when used as a lighting material.
4. The material disclosed by the invention is simple in preparation process and low in cost, can be synthesized in one step at relatively low reaction temperature only by a hydrothermal method, and is high in feasibility of industrialization.
Drawings
FIG. 1 is an emission spectrum of a sample of example 1 under 365nm excitation;
FIG. 2 is an emission spectrum of a sample of example 2 under 365nm excitation;
FIG. 3 is the emission spectrum of the sample of example 3 under 365nm excitation;
FIG. 4 is an emission spectrum of a sample of comparative example 1 under 365nm excitation;
FIG. 5 shows example 1
Example 2 (. diamond-solid.), example 3
Comparative example 1
The chromaticity coordinates of the sample;
FIG. 6 is a temperature-variable fluorescence spectrum of a sample of example 1;
figure 7 is an XRD pattern of the sample of example 1.
Figure 8 is an XRD pattern of the sample of comparative example 2.
Detailed Description
The invention is further described below with reference to the figures and examples, without limiting the scope of the invention to these.
Example 1
The chemical formula of the sample in this example is Cs 2 Sn 0.6 Te 0.3 Bi 0.1 Cl 6 . According to the proportion of each element in the chemical formula, the medicine is determined as follows: 2mmol CsCl,0.6mmol SnCl 2 ,0.3mmol TeO 2 ,0.05mmol Bi 2 O 3 。
(1) Each drug was weighed out with 5mL of concentrated hydrochloric acid (mass fraction: about 37%) and poured into a stainless steel reaction kettle lined with teflon.
(2) And (3) placing the sealed stainless steel reaction kettle in a muffle furnace, and carrying out heat treatment at 180 ℃ for 12 h.
(3) And (3) cooling the stainless steel reaction kettle to room temperature in a muffle furnace at a cooling rate of less than 5 ℃/h.
(4) And filtering the mixture in the reaction kettle to obtain precipitates, washing the precipitates with acetone, absolute ethyl alcohol and deionized water respectively, and then naturally drying the precipitates to obtain the target product.
FIG. 7 is an XRD pattern of the sample of example 1, which, when compared to a standard card, shows that the sample after double doping still retains Cs 2 SnCl 6 The crystal structure of double perovskite. Fig. 1 is an emission spectrum of the sample of example 1 under 365nm excitation, which is mainly composed of two emission peaks in the visible light range, respectively a blue light emission peak at a peak position around 460nm (FWHM ═ 70nm) and a yellow light emission peak at a peak position around 570nm (FWHM ═ 119 nm). From FIG. 5
It can be seen that his chromaticity coordinates are (0.33,0.36), a warm white light very close to the isoenergetic white point. FIG. 6 is a temperature-variable fluorescence spectrum of a sample of example 1, wherein although the fluorescence intensity of the material decreases with increasing temperature, no color shift occurs, indicating that the fluorescence of the material has better thermal stability.
Example 2
The chemical formula of the sample in this example is Cs 2 Sn 0.65 Te 0.3 Bi 0.05 Cl 6 . According to the proportion of each element in the chemical formula, the medicine is determined as follows: 2mmol CsCl,0.65mmol SnCl 2 ,0.3mmol TeO 2 ,0.025mmol Bi 2 O 3 。
(1) Each drug was weighed out with 5mL of concentrated hydrochloric acid (mass fraction: about 37%) and poured into a stainless steel reaction kettle lined with teflon.
(2) And (3) placing the sealed stainless steel reaction kettle in a muffle furnace, and carrying out heat treatment at 180 ℃ for 12 h.
(3) And (3) cooling the stainless steel reaction kettle to room temperature in a muffle furnace at a cooling rate of less than 5 ℃/h.
(4) And filtering the mixture in the reaction kettle to obtain precipitates, washing the precipitates with acetone, absolute ethyl alcohol and deionized water respectively, and then naturally drying the precipitates to obtain the target product.
Fig. 2 is an emission spectrum of the sample of example 2 under 365nm excitation, which is mainly composed of two emission peaks in the visible light range, respectively a blue light emission peak with a peak position around 460nm (FWHM of 64nm) and a yellow light emission peak with a peak position around 570nm (FWHM of 112 nm). From FIG. 5 (. diamond-solid.) it can be seen that his chromaticity coordinates are (0.36,0.39), which is a warm white light.
Example 3
The chemical formula of the sample in this example is Cs 2 Sn 0.5 Te 0.3 Bi 0.2 Cl 6 . According to the proportion of each element in the chemical formula, the medicine is determined as follows: 2mmol CsCl,0.5mmol SnCl 2 ,0.3mmol TeO 2 ,0.1mmol Bi 2 O 3 。
(1) Each drug was weighed out with 5mL of concentrated hydrochloric acid (mass fraction: about 37%) and poured into a stainless steel reaction kettle lined with teflon.
(2) And (3) placing the sealed stainless steel reaction kettle in a muffle furnace, and carrying out heat treatment at 180 ℃ for 12 h.
(3) And (3) cooling the stainless steel reaction kettle to room temperature in a muffle furnace at a cooling rate of less than 5 ℃/h.
(4) And filtering the mixture in the reaction kettle to obtain precipitates, washing the precipitates with acetone, absolute ethyl alcohol and deionized water respectively, and then naturally drying the precipitates to obtain the target product.
Fig. 3 is an emission spectrum of the sample of example 3 under 365nm excitation, which is mainly composed of two emission peaks in the visible light range, respectively a blue light emission peak with a peak position around 460nm (FWHM ═ 63nm) and a yellow light emission peak with a peak position around 570nm (FWHM ═ 96 nm). From fig. 5, it can be seen that his chromaticity coordinates are (0.27,0.30), which is a cool white light.
Comparative example 1
The sample of this comparative example has the chemical formula Cs 2 Sn 0.69 Te 0.3 Bi 0.01 Cl 6 . According to the proportion of each element in the chemical formula, the medicine is determined as follows: 2mmol CsCl,0.69mmol SnCl 2 ,0.3mmol TeO 2 ,0.005mmol Bi 2 O 3 。
(1) Each drug was weighed out with 5mL of concentrated hydrochloric acid (mass fraction: about 37%) and poured into a stainless steel reaction kettle lined with teflon.
(2) And (3) placing the sealed stainless steel reaction kettle in a muffle furnace, and carrying out heat treatment at 180 ℃ for 12 h.
(3) And (3) cooling the stainless steel reaction kettle to room temperature in a muffle furnace at a cooling rate of less than 5 ℃/h.
(4) And filtering the mixture in the reaction kettle to obtain precipitates, washing the precipitates with acetone, absolute ethyl alcohol and deionized water respectively, and then naturally drying the precipitates to obtain the target product.
Fig. 4 is an emission spectrum of the sample of comparative example 1 under 365nm excitation, which is mainly composed of two emission peaks in the visible light range, respectively a blue light emission peak at a peak position around 460nm (FWHM 67nm) and a yellow light emission peak at a peak position around 570nm (FWHM 117 nm). From fig. 5, it can be seen that his chromaticity coordinates are (0.38,0.42), which is a yellow light.
Comparative example 2
The initial drug composition of the sample of this comparative example was: 2mmol CsCl,0.725mmol SnCl 2 ,0.1375mmol Bi 2 O 3 。
(1) Each drug was weighed out with 5mL of concentrated hydrochloric acid (mass fraction: about 37%) and poured into a stainless steel reaction kettle lined with teflon.
(2) And (3) placing the sealed stainless steel reaction kettle in a muffle furnace, and carrying out heat treatment at 180 ℃ for 12 h.
(3) And (3) cooling the stainless steel reaction kettle to room temperature in a muffle furnace at a cooling rate of less than 5 ℃/h.
(4) And filtering the mixture in the reaction kettle to obtain precipitates, washing the precipitates with acetone, absolute ethyl alcohol and deionized water respectively, and then naturally drying the precipitates to obtain the target product.
Because the valence states of Bi and Sn are different and the ionic radius difference is larger, the solid solubility of Bi in solid solution is smaller when y is larger>At 0.22, a hetero-phase will appear in the product from the reaction. FIG. 8 is an XRD pattern of comparative example 2, and it can be confirmed by phase analysis that too high Bi content causes Cs to be formed in the material 3 Bi 2 Cl 9 A hetero-phase of an orthorhombic system.
Claims (7)
1. A single-phase fluorescent material for white light LED is characterized in thatIn the following steps: the single-phase fluorescent material for the white light LED consists of single-phase solid solution, and the molecular formula of the single-phase solid solution is Cs 2 Sn 1-x-y Te x Bi y Cl 6 X =0.3, y is in the value range of 0.05-0.22.
2. The method for preparing a single-phase fluorescent material for a white LED as claimed in claim 1, wherein the method comprises the following steps: and mixing the Cs source, the Sn source, the Te source, the Bi source and hydrochloric acid according to a set molar ratio, and carrying out hydrothermal reaction to obtain the single-phase fluorescent material for the white light LED.
3. The production method according to claim 2, characterized in that: the Cs source is CsCl; the Sn source is SnCl 2 、SnCl 2 ·2H 2 O or SnCl 4 (ii) a The Te source is TeO 2 Or TeCl 4 (ii) a The source of Bi is Bi 2 O 3 Or BiCl 3 。
4. The method of claim 2, wherein: the hydrochloric acid is concentrated hydrochloric acid with the mass fraction of 36-38%.
5. The method of claim 2, wherein: the temperature of the hydrothermal reaction is 150-200 ℃; the time is 5-18 h.
6. The method of claim 2, wherein: the temperature reduction rate after the hydrothermal reaction is not higher than 5 ℃/h.
7. The use of the single-phase fluorescent material for white LED according to claim 1 or the single-phase fluorescent material for white LED prepared by the preparation method according to any one of claims 2 to 6, wherein: it is used for manufacturing a light emitting device.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108659827A (en) * | 2018-06-15 | 2018-10-16 | 华中科技大学 | Near ultraviolet excitated double-perovskite single-substrate white fluorescent material and preparation and application |
| CN110803711A (en) * | 2019-11-18 | 2020-02-18 | 桂林电子科技大学 | Te doped A2SnCl6Perovskite material and preparation method thereof |
| CN111876156A (en) * | 2020-06-03 | 2020-11-03 | 华中科技大学 | White light fluorescent powder and preparation method and application thereof |
| CN112794362A (en) * | 2020-12-25 | 2021-05-14 | 清华-伯克利深圳学院筹备办公室 | Inorganic perovskite material, preparation method thereof and LED device |
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| CN108659827A (en) * | 2018-06-15 | 2018-10-16 | 华中科技大学 | Near ultraviolet excitated double-perovskite single-substrate white fluorescent material and preparation and application |
| CN110803711A (en) * | 2019-11-18 | 2020-02-18 | 桂林电子科技大学 | Te doped A2SnCl6Perovskite material and preparation method thereof |
| CN111876156A (en) * | 2020-06-03 | 2020-11-03 | 华中科技大学 | White light fluorescent powder and preparation method and application thereof |
| CN112794362A (en) * | 2020-12-25 | 2021-05-14 | 清华-伯克利深圳学院筹备办公室 | Inorganic perovskite material, preparation method thereof and LED device |
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| Title |
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| Ruosheng Zeng et al.,.Boosting triplet self-trapped exciton emission in Te(IV)-doped Cs2SnCl6 perovskite variants.《Nano Res.》.2020,第1551-1558页. * |
| Zhifang Tan et al.,.Highly Efficient Blue-Emitting Bi-Doped Cs2SnCl6 Perovskite Variant: Photoluminescence Induced by Impurity Doping.《Adv. Funct. Mater.》.2018,第28卷第1801131：1-10页. * |
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