CN116023941A - Near infrared fluorescent powder and preparation method and application thereof - Google Patents
Near infrared fluorescent powder and preparation method and application thereof Download PDFInfo
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- CN116023941A CN116023941A CN202211742155.3A CN202211742155A CN116023941A CN 116023941 A CN116023941 A CN 116023941A CN 202211742155 A CN202211742155 A CN 202211742155A CN 116023941 A CN116023941 A CN 116023941A
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- 239000000843 powder Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 18
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000000295 emission spectrum Methods 0.000 claims description 4
- 238000000695 excitation spectrum Methods 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000001228 spectrum Methods 0.000 abstract description 8
- 230000005284 excitation Effects 0.000 abstract description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 7
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000007599 discharging Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 229910004261 CaF 2 Inorganic materials 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 108010043121 Green Fluorescent Proteins Proteins 0.000 description 1
- 101100476480 Mus musculus S100a8 gene Proteins 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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Abstract
The application discloses near infrared fluorescent powder, a preparation method and application thereof, and relates to the technical field of luminescent materials, wherein the chemical general formula of the near infrared fluorescent powder is as follows: MAl 12‑x‑y Ga y O 19‑Z F Z :xCr 3+ Wherein M is selected from at least one of Ca element, sr element, ba element or Mg element, and M at least contains Ca element; x is more than or equal to 0.05 and less than or equal to 0.2; y is more than or equal to 3 and less than or equal to 12; the value range of z is more than or equal to 0.01 and less than or equal to 0.1. The near infrared fluorescent powder has the main emission peak of 750-830 nm, and can be generally used in the prior artThe blue light or purple light LED chip with the excitation peak wavelength of 400-500 nm is used for excitation, the spectrum coverage within the range of 700nm is realized, the luminous efficiency is high, and the internal quantum efficiency of the fluorescent powder can reach more than 80%.
Description
Technical Field
The application relates to the technical field of luminescent materials, in particular to near infrared fluorescent powder and a preparation method and application thereof.
Background
In the field of full spectrum LED illumination, a blue LED chip, blue-green fluorescent powder, green fluorescent powder and red fluorescent powder are generally used as a fluorescent powder combination scheme to realize a full spectrum white light LED with a color rendering index of more than 97, but the full spectrum white light LED lacks efficient spectrum coverage in a range after 700 nm. The related art discloses a red phosphor, the chemical composition of which has the general formula of Al 12 O 19 :Cr 3+ The emission wavelength is 685nm, belongs to dark red fluorescent powder, but has limited coverage of near infrared emission bands, and when the fluorescent powder is used as combined fluorescent powder, the spectrum cannot truly cover the full visible light band of 400-780 nm, and the coverage of the near infrared band of 780-900nm cannot be realized.
Disclosure of Invention
The application provides near infrared fluorescent powder, a preparation method and application thereof, wherein the emission main peak of the near infrared fluorescent powder is between 750 and 830nm, the near infrared fluorescent powder can be excited by a blue or purple light LED chip commonly used in the prior art, the spectrum coverage within the range of 700nm is realized, the luminous efficiency is high, and the internal quantum efficiency of the fluorescent powder can reach more than 80%.
In a first aspect, the present application provides a near infrared phosphor selected from any one of the substances having formula i; MAl 12-x-y Ga y O 19-Z F Z :xCr 3+ Wherein M is selected from at least one of Ca element, sr element, ba element or Mg element, and M at least contains Ca element; x is more than or equal to 0.05 and less than or equal to 0.2; y is more than or equal to 3 and less than or equal to 12; the value range of z is more than or equal to 0.001 and less than or equal to 0.1.
MAl 12-x O 19 :xCr 3+ In the phosphor, cr replaces Al element, but the difference of ionic radii of Al element and Cr element is larger, so that larger lattice distortion is generated, the crystallization performance of the phosphor crystal is deteriorated, and MAl is added 12-x O 19 Modification of matrix crystals to MAl 12-y Ga y O 19 The matrix crystal, at this time, the Cr element is replaced by Ga element with a closer ionic radius, so that the lattice distortion phenomenon is greatly improved, and the luminous performance is greatly improved. At the same time, by further adding to MAl 12-y Ga y O 19 A small amount of F element is introduced into the matrix, so that the luminous brightness of the fluorescent powder is further improved.
It should be noted that, the content of each element in the substance shown in the formula I also needs to satisfy a certain range, for example, when the content y of Ga element is lower than 3, the luminescence wavelength of the fluorescent powder is shorter than 750nm, and the luminescence efficiency is low; when the content x of Cr element is lower than 0.05, the luminous efficiency is low due to too few luminous centers in the fluorescent powder particles, but when x is higher than 0.2, serious quenching phenomenon of the luminous center concentration is caused, and the luminous efficiency of the fluorescent powder is also obviously reduced; when the content z of the F element is higher than 0.1, the fluorescent powder particles are excessively grown and large, and meanwhile, serious adhesion phenomenon is generated, so that the application of the fluorescent powder is not facilitated. Therefore, the element content is controlled in a proper range, which is beneficial to improving the luminous efficiency of the fluorescent powder.
Illustratively, x may have any value in the range of 0.05, 0.06, 0.07, 0.09, 0.1, 0.13, 0.15, 0.18, 0.2.
Illustratively, y may have any of values 3, 4, 5, 6, 7, 8, 9, 10, 11, 12.
Illustratively, z may have any value in the range of 0.01, 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1.
In some embodiments, x is in the range of 0.1.ltoreq.x.ltoreq.0.15. At this time, the content range of Cr element is suitable, which is advantageous for improving the luminous efficiency.
Illustratively, x may have a value in any of the values 0.1, 0.11, 0.12, 0.13, 0.14, 0.15.
In some embodiments, y has a value in the range of 4.ltoreq.y.ltoreq.5. At this time, the luminescence property of the phosphor is better.
Illustratively, y may have a value in the range of any of 4, 4.2, 4.4, 4.5, 4.7, 4.8, 5.
In some embodiments, z has a value in the range of 0.05.ltoreq.z.ltoreq.0.1. At the moment, the content of the F element is proper, and the prepared fluorescent powder particles are moderate in size, so that the subsequent application of the fluorescent powder is facilitated.
In some of these embodiments, the following are satisfied: x is more than or equal to 0.1 and less than or equal to 0.15,4, y is more than or equal to 5 and z is more than or equal to 0.05 and less than or equal to 0.1. At this time, the internal quantum efficiency of the prepared fluorescent powder is highest, which is more beneficial to the further application of the fluorescent powder.
In some of these embodiments, the near infrared phosphor has an emission spectrum covering a wavelength range of 750 to 830nm.
In some of these embodiments, the near infrared phosphor has an excitation spectrum covering a wavelength range of 400 to 500nm. It can be seen that the near infrared phosphor can be effectively excited by blue light or violet light in the range of 400-500 nm.
In some of these embodiments, the near infrared phosphor has an average particle size of 10-25 μm.
In a second aspect, the present application provides a method for preparing the above near infrared fluorescent powder, including the following steps:
(1) Per MAl 12-x-y Ga y O 19-Z F Z :xCr 3+ Weighing M source, al source, ga source, cr source and NH according to the chemical dose ratio 4 F or MF 2 Mixing to obtain a mixture;
wherein the M source contains at least one of Ca element, sr element, ba element or Mg element, and MF 2 Preferably CaF 2 ；
(2) Under the air atmosphere or inert gas atmosphere, the mixture is burned for 1 to 10 hours at 1450 to 1600 ℃ and burned at least once to obtain a burned product;
(3) And grinding the firing product, and washing and drying to obtain the near infrared fluorescent powder.
In some embodiments, the M source is a carbonate containing M element, the Al source is an oxide containing Al element, the Ga source is an oxide containing Ga element, and the Cr source is an oxide containing Cr element.
Specifically, the carbonate containing M element can be CaCO 3 The oxide containing Al element can be Al 2 O 3 The oxide containing Ga element can be Ga 2 O 3 The oxide containing Cr element can be Cr 2 O 3 。
In a third aspect, the application provides application of the near infrared fluorescent powder in plant illumination and food detection.
The technical scheme provided by some embodiments of the present application has the beneficial effects that at least includes: the application provides near infrared fluorescent powder, wherein the main emission peak of the near infrared fluorescent powder is between 750 and 830nm, the near infrared fluorescent powder can be excited by a blue or violet LED chip with the excitation peak wavelength of 400 to 500nm commonly used in the prior art, the spectrum coverage within the range of 700nm is realized, the luminous efficiency is high, the quantum efficiency in the fluorescent powder is up to more than 80%, and the maximum is about 90%.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a chart showing the excitation spectrum of the near infrared phosphor of example 1 of the present application;
FIG. 2 is a graph showing the emission spectrum of the near infrared phosphor of example 1 of the present application;
fig. 3 is a scanning electron microscope image of the near infrared phosphor of example 1 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be further described in detail with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the present application.
The present application is further illustrated by the following examples.
Example 1
CaAl according to chemical composition 8.95 Ga 3 O 18.99 F 0.01 :0.05Cr 3+ Weighing the raw materials with the corresponding weight: 100.1g CaCO 3 ，292g Ga 2 O 3 、456.3g Al 2 O 3 、3.8g Cr 2 O 3 0.37g NH F; mixing the materials, heating to 1450 ℃ in a muffle furnace in air atmosphere, burning for 10 hours, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The main emission peak of the near infrared fluorescent powder is 750nm; the internal quantum efficiency was 83.2%.
FIG. 1 is a chemical formula CaAl in example 1 of the present application 8.95 Ga 3 O 18.99 F 0.01 :0.05Cr 3+ As can be seen from fig. 1, the excitation spectrum of the near infrared phosphor has a main peak covering a wavelength range of 400-500 nm, and can be excited by a blue or violet chip commonly used in the prior art.
FIG. 2 is a chemical formula CaAl in example 1 of the present application 8.95 Ga 3 O 18.99 F 0.01 :0.05Cr 3+ As can be seen from fig. 2, the emission spectrum of the near infrared phosphor achieves spectral coverage in the range of 700nm and has high luminous efficiency.
FIG. 3 is a chemical formula CaAl in example 1 of the present application 8.95 Ga 3 O 18.99 F 0.01 :0.05Cr 3+ Scanning Electron Microscope (SEM) of the near infrared phosphor, it can be seen from fig. 3 that the near infrared phosphor particles are distributed more uniformly and have a proper particle size.
Example 2
CaAl according to chemical composition 7.9 Ga 4 O 18.95 F 0.05 :0.1Cr 3+ Weighing the raw materials with the corresponding weight: 100.1g CaCO 3 ，389.3g Ga 2 O 3 、402.7g Al 2 O 3 、7.6g Cr 2 O 3 1.85g NH F; mixing the above materials, and placing in N 2 Heating to 1510 ℃ in a muffle furnace in atmosphere, burning for 4 hours, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The main emission peak of the near infrared fluorescent powder is 780nm; the internal quantum efficiency is 89.3%.
Example 3
CaAl according to chemical composition 6.85 Ga 5 O 18.9 F 0.1 :0.15Cr 3+ Weighing the raw materials with the corresponding weight: 95.1g CaCO 3 ，486.6g Ga 2 O 3 、349.2g Al 2 O 3 、11.4g Cr 2 O 3 3.9g CaF 2 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the materials, heating to 1600 ℃ in a muffle furnace in air atmosphere, burning for 1h, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The emission main peak of the near infrared fluorescent powder is 795nm; the internal quantum efficiency is 86.3%.
Example 4
CaAl according to chemical composition 2.85 Ga 9 O 18.95 F 0.05 :0.15Cr 3+ Weighing the raw materials with the corresponding weight: 97.6g CaCO 3 ，875.9g Ga 2 O 3 、145.3g Al 2 O 3 、11.4g Cr 2 O 3 1.95g CaF 2 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the above materials, and placing in N 2 Heating to 1500 ℃ in a muffle furnace in atmosphere, burning for 6h, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The main emission peak of the near infrared fluorescent powder is at 815nm; the internal quantum efficiency is 82.7%.
Example 5
According to chemical composition CaGa 11.8 O 18.95 F 0.05 :0.2Cr 3+ Weighing the raw materials with the corresponding weight: 97.6g CaCO 3 ，1167.8g Ga 2 O 3 、11.4g Cr 2 O 3 1.95g CaF 2 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the above materials, and placing in N 2 Heating to 1470 ℃ in a muffle furnace in atmosphere, burning for 8 hours, cooling to room temperature along with the furnace, and discharging; will beThe firing product is obtained after ball milling, washing and drying. The main emission peak of the near infrared fluorescent powder is 830nm; the internal quantum efficiency is 80.7%.
Example 6
According to chemical composition Ca 0.5 S r0.4 Mg 0.1 Al 0.1 Ga 11.8 O 18.975 F 0.025 :0.1Cr 3+ Weighing the raw materials with the corresponding weight: 48.8g CaCO 3 ，57.6g SrCO 3 ，3.9g MgO，1148.4g Ga 2 O 3 、5.1g Al 2 O 3 、5.7g Cr 2 O 3 0.93g NH F; mixing the materials, heating to 1450 ℃ in a muffle furnace in air atmosphere, burning for 10 hours, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The main emission peak of the near infrared fluorescent powder is at 825m; the internal quantum efficiency is 81.2%.
Comparative example 1
CaAl according to chemical composition 11.9 O 19 :0.1Cr 3+ Weighing the raw materials with the corresponding weight: 100.1g CaCO 3 ，611.8g Al 2 O 3 、7.6g Cr 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the Mixing the above materials, and placing in N 2 Heating to 1510 ℃ in a muffle furnace in atmosphere, burning for 4 hours, cooling to room temperature along with the furnace, and discharging; and ball milling, washing and drying the firing product. The main emission peak of the near infrared fluorescent powder is at 710nm; the internal quantum efficiency is 55.4%.
TABLE 1
As can be seen from Table 1, the compounds have the chemical formula MAl shown in the application 12-x-y Ga y O 19-Z F Z :xCr 3+ Compared with MAl in the prior art 12-x O 19 :xCr 3+ The fluorescent powder has narrower half peak width and better luminous performance, especially the values of x, y and z are set in proper ranges, thus being beneficial to further improving the luminous performance and the internal quantum efficiency of the fluorescent powder can be improvedApproximately 90%.
The foregoing description of the preferred embodiments of the present application is not intended to be limiting, but is intended to cover any and all modifications, equivalents, and alternatives falling within the spirit and principles of the present application.
Claims (10)
1. The near infrared fluorescent powder is characterized in that the near infrared fluorescent powder is selected from any one of substances shown in a formula I;
MAl 12-x-y Ga y O 19-Z F Z :xCr 3+ i
Wherein M is selected from at least one of Ca element, sr element, ba element or Mg element, and M at least contains Ca element;
x is more than or equal to 0.05 and less than or equal to 0.2;
y is more than or equal to 3 and less than or equal to 12;
the value range of z is more than or equal to 0.01 and less than or equal to 0.1.
2. The near infrared phosphor of claim 1, wherein in the formula i, at least one of the following conditions is satisfied:
condition I: x is more than or equal to 0.1 and less than or equal to 0.15;
condition II: y is more than or equal to 4 and less than or equal to 5;
condition III: the value range of z is more than or equal to 0.05 and less than or equal to 0.1.
3. The near infrared phosphor of claim 1, wherein the emission spectrum of the near infrared phosphor covers a wavelength range of 750 to 830nm.
4. The near infrared phosphor of claim 1, wherein the excitation spectrum of the near infrared phosphor covers a wavelength range of 400 to 500nm.
5. The near infrared phosphor of claim 1, wherein the near infrared phosphor has an average particle size of 10-25 μm.
6. The method for preparing near infrared phosphor according to any one of claims 1 to 5, comprising the steps of:
(1) Per MAl 12-x-y Ga y O 19-Z F Z :xCr 3+ Weighing M source, al source, ga source, cr source and NH according to the chemical dose ratio 4 F or MF 2 Mixing to obtain a mixture;
(2) Under the air atmosphere or inert gas atmosphere, the mixture is burned for 1 to 10 hours at 1450 to 1600 ℃ and burned at least once to obtain a burned product;
(3) And grinding, washing and drying the firing product to obtain the near infrared fluorescent powder.
7. The method according to claim 6, wherein the M source is a carbonate containing an element M, the Al source is an oxide containing an element Al, the Ga source is an oxide containing an element Ga, and the Cr source is an oxide containing an element Cr.
8. Use of the near infrared phosphor of any one of claims 1 to 5 for plant illumination and food detection.
9. A lighting device comprising the near infrared phosphor of any one of claims 1 to 5.
10. A food detection device comprising the near infrared phosphor of any one of claims 1 to 5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971468A (en) * | 2019-03-18 | 2019-07-05 | 广东工业大学 | A kind of long-persistence nano material and its preparation method and application |
| US20200048549A1 (en) * | 2017-05-11 | 2020-02-13 | Mitsubishi Chemical Corporation | Light emitting device and phosphor |
| CN113088286A (en) * | 2021-03-23 | 2021-07-09 | 北京科技大学 | Ytterbium-containing near-infrared ultra-long afterglow gallate luminescent material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200048549A1 (en) * | 2017-05-11 | 2020-02-13 | Mitsubishi Chemical Corporation | Light emitting device and phosphor |
| CN109971468A (en) * | 2019-03-18 | 2019-07-05 | 广东工业大学 | A kind of long-persistence nano material and its preparation method and application |
| CN113088286A (en) * | 2021-03-23 | 2021-07-09 | 北京科技大学 | Ytterbium-containing near-infrared ultra-long afterglow gallate luminescent material and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 禹德朝;张勤远;: "近红外量子剪裁研究进展", 中国科学:化学, no. 11 * |
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