CN117586774A - Cr (chromium) 3+ Doped broadband near infrared fluorescent powder and application thereof - Google Patents
Cr (chromium) 3+ Doped broadband near infrared fluorescent powder and application thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 67
- 239000011651 chromium Substances 0.000 title claims description 40
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims description 4
- 229910052804 chromium Inorganic materials 0.000 title claims description 4
- 230000005284 excitation Effects 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 3
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 238000000295 emission spectrum Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000002223 garnet Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 2
- 229910017855 NH 4 F Inorganic materials 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005286 illumination Methods 0.000 abstract description 6
- 230000004297 night vision Effects 0.000 abstract description 5
- 238000003384 imaging method Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 description 12
- 239000007787 solid Substances 0.000 description 6
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 5
- 229910005793 GeO 2 Inorganic materials 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 238000005090 crystal field Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K11/7707—Germanates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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Abstract
The invention discloses a Cr 3+ Doped broadband near infrared fluorescent powder and application thereof, wherein the chemical general formula of the fluorescent powder is A1 3‑ y A2 y B 2‑x C1 y C2 3‑y O 12 :xCr 3+ (0 < y < 3,0 < x.ltoreq.0.14), wherein a1= Ca, mg, ba, cd, sr, zn; a2 = Y, gd, la, in; b=c1= Al, ga, sc, lu; c2 = Ge, si, ti, hf, zr. The fluorescent powder has larger composition selection and adjustment scope and good thermal stability. The fluorescent powder is prepared by adopting a high-temperature solid-phase sintering method, has a wider excitation light wavelength range, can be applied to a near-infrared LED light source, is very suitable for blue LED excitation, can realize near-infrared emission with a half-peak width of 95-153 nm and high internal quantum efficiency and thermal stability, and can be widely applied to the fields of plant illumination, night vision imaging and the like.
Description
Technical Field
The invention belongs to luminescence fluorescenceThe technical field of light powder, in particular to a Cr 3+ The doped broadband near infrared fluorescent powder is used as a near infrared luminescent material of a conversion LED and is applied to the fields of plant illumination and night vision imaging.
Background
Near infrared light has the advantages of low energy, strong penetrating power and the like, so that the near infrared spectrum technology integrates the characteristics of high detection speed, no damage, real time and the like, is more and more concerned, and has huge application prospects in the fields of detection analysis, biological imaging, night vision illumination, modern agriculture, machine vision and the like. The near infrared light sources commonly used in the market mainly comprise incandescent lamps, halogen lamps, fluorescent lamps, short wave infrared lasers and infrared light emitting diodes, which all have inherent drawbacks. Incandescent lamps and halogen lamps are bulky, high in energy consumption, low in efficiency, and short in service life; the fluorescent lamp has low efficiency, contains heavy metal elements and is easy to flash; the short wave infrared laser has small divergence angle, high power consumption and relatively high cost; the infrared light-emitting diode has narrower emission band, poor thermal stability and high production equipment cost, and can not be widely applied to the technical field of near infrared spectrum.
With the rapid development and wide application of the white light LED technology, the fluorescent powder conversion type light emitting device combining the commercial high-power blue light LED chip and the near infrared light emitting material is becoming an ideal choice of a new generation solid near infrared light source by referring to the developed and mature fluorescent powder conversion white light LED technology. Therefore, development of a phosphor capable of being efficiently excited by a blue LED and converting it into near infrared light is important for development of a novel phosphor-converted near infrared LED having low cost and high luminous efficiency.
Cr 3+ The outermost electron configuration of (2) is 3d 3 ， 4 T 2g → 4 A 2g The energy of the transition is subject to Cr 3+ The field intensity of the octahedral crystal is influenced, and broadband near infrared emission is easy to generate in the weak octahedral field. The garnet structure material has a rigid structure, and can realize the regulation and control of the environment of the ion crystal field of the luminescence center easily through the component design of ion substitution, thereby realizing the spectrum regulation and control. Cr (Cr) 3+ Single doping and Cr 3+ /Mn 2+ Co-doped Ca 3 Al 2 Ge 3 O 12 Near infrared phosphors have been reported to Cr under efficient excitation of blue light 3+ Is located at 722 nm. To further increase Cr 3+ The comprehensive performance of the doped garnet structure near-infrared LED is significant in developing novel near-infrared fluorescent powder with high luminous efficiency, wide emission spectrum and high thermal stability by adopting a proper substitution strategy.
The patent discloses a novel Cr 3+ The doped broadband near infrared fluorescent powder has the advantages of wide emission spectrum, adjustable emission wavelength, high luminous efficiency, good thermal stability and the like, and is expected to be applied to plant factory illumination LEDs, night vision illumination and the like.
Disclosure of Invention
The invention aims to provide Cr which can be effectively excited by blue light 3+ The invention adjusts the crystal field intensity of octahedron and reduces the symmetry thereof by carrying out chemical co-substitution on dodecahedron and tetrahedron in the garnet structure, thereby adjusting Cr 3+ Is a light-emitting property of (a) a light-emitting element. The fluorescent powder can be effectively excited by blue light, and has high luminous efficiency and wide band range.
In order to achieve the above purpose, the invention adopts the following technical scheme:
cr (chromium) 3+ Doped broadband near infrared fluorescent powder with a chemical general formula of A1 3-y A2 y B 2-x C1 y C2 3-y O 12 :xCr 3+ (0 < y < 3,0 < x.ltoreq.0.14), wherein a1= Ca, mg, ba, cd, sr, zn; a2 = Y, gd, la, in; b=c1= Al, ga, sc, lu; c2 = Ge, si, ti, hf, zr. With Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ For example, the excitation peak is 450nm, the emission peak is 780nm, the full width at half maximum (FWHM) is 149nm, the Internal Quantum Efficiency (IQE) and the External Quantum Efficiency (EQE) are respectively 84.4% and 45.9%, and the ratio I of the integrated luminous intensity at 300K to the integrated luminous intensity at 423K 423 k /I 300 k =80.38% withHas high thermal stability, and the highest photoelectric conversion efficiency is 15.8%.
Preferably, in the chemical formula, B and C1 are homologous elements, occupy octahedral sites and tetrahedral sites, respectively, and have an ionic radius of B and C1 greater than C2; a1 and A2 occupy dodecahedral sites and have an ionic radius greater than B and C1.
The invention also provides Cr 3+ The preparation method of the doped broadband near infrared fluorescent powder adopts a high-temperature solid phase sintering method, and comprises the following specific steps:
(a) Weighing the corresponding oxides or carbonates of A1, A2, B, C1 and C2 according to the molecular formula of the fluorescent powder, fully mixing, adding a certain amount of fluxing agent, and grinding uniformly;
(b) Loading the mixture obtained in the step (a) into a corundum crucible or a graphite crucible, transferring the corundum crucible or the graphite crucible into a tube furnace, sintering at a certain temperature, preserving heat for a period of time, and then cooling to room temperature;
(c) Fully grinding the sintered product obtained in the step (b) to obtain a novel Cr 3+ A broadband near infrared fluorescent powder doped with garnet structure.
Preferably, in step (a), the fluxing agent is B 2 O 3 、Li 2 CO 3 、CaF 2 、P 2 O 5 、LiF、NH 4 F、K 2 CO 3 One or more of the following; the added content is 1-7wt% of the total mass of the fluorescent powder synthetic raw material.
Preferably, in step (b), the number of sintering is one or more.
Preferably, in the step (b), the temperature rising rate is 3-10 ℃/min, the roasting temperature is 700-1600 ℃, and the single roasting time is 3-8 h.
The invention further provides a Cr 3+ Application of doped broadband near infrared fluorescent powder, cr 3+ The doped broadband near infrared fluorescent powder is applied to a near infrared LED light source, has broadband near infrared luminescence under 450nm light excitation, has an emission spectrum between 650 and 1150nm, a half-peak width between 95 and 153nm, and has an internal quantum efficiency of 84.4% at the maximum, and fluorescent powder at 423K temperatureThe luminous intensity of the fluorescent lamp keeps 80.4% of room temperature, and can be widely applied to the fields of plant illumination, night vision imaging and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) The fluorescent powder has larger composition selection and adjustment scope and good thermal stability.
(2) The fluorescent powder has a relatively wide excitation light wavelength range and has the strongest excitation peak at about 450nm, so that the fluorescent powder is very suitable for blue light LED excitation.
(3) The preparation method of the fluorescent powder is feasible, has simple production flow and is convenient for large-scale production.
(4) The LED light source can realize near infrared emission with wide band (half-peak width is 95-153 nm), high efficiency (internal quantum efficiency can reach 84.4%), and high thermal stability (the luminous intensity of the fluorescent powder keeps 84.4% of the luminous intensity at room temperature at 423K).
Drawings
FIG. 1 is Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ XRD pattern of (c) and Ca 3 Al 2 Ge 3 O 12 Standard card (PDF # 10-0265).
FIG. 2 is Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ Is a scanning electron microscope image of (1).
FIG. 3 is Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ An excitation spectrum and an emission spectrum of the same.
FIG. 4 is a view of Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ And (3) an emission spectrum diagram of the pc-LED packaged by the fluorescent powder and the blue LED chip under different currents.
Detailed Description
Example 1
Cr 3+ Garnet-structure-doped broadband near infrared fluorescent powder Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ Is green solid powder, and the preparation method is as follows:
(1) Weighing CaCO according to stoichiometric ratio 3 :0.1g，Y 2 O 3 :0.05645g，Al 2 O 3 :0.07515g，GeO 2 :0.10459g，Cr 2 O 3 0.0019g. The raw materials are fully mixed and ground uniformly.
(2) Dividing the obtained mixture into two parts, respectively loading into corundum crucibles, transferring into a tube furnace, performing two groups of roasting experiments, heating the mixture to 1000 ℃ at a heating rate of 5 ℃/min, heating the mixture to 1450 ℃ at a heating rate of 2 ℃/min, and preserving heat for 6 hours; the second group of roasting experiments are heated to 1000 ℃ at a heating rate of 5 ℃/min, and then heated to 1400 ℃ at a heating rate of 2 ℃/min for 6h; then cooling to room temperature at a cooling rate of 2 ℃/min.
(3) Fully grinding the sintered product obtained in the step (2) for 3min to obtain Cr 3+ Doped garnet-structured broadband near infrared fluorescent powder Ca 2 Y 1 Al 2.95 Ge 2 O 12 :0.05Cr 3+ 。
FIG. 1 is a XRD spectrum of a near infrared phosphor obtained by a first set of firing experiments, in which it can be seen that the diffraction peaks of the phosphor and Ca of garnet structure 3 Al 2 Ge 3 O 12 The diffraction peaks of the (PDF # 10-0265) standard card correspond well, indicating that the phosphor is also garnet structure and has good crystallinity.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the near infrared phosphor obtained in the first set of firing experiments, and it can be seen that the obtained phosphor is a smooth surface but irregular micron-sized phosphor.
FIG. 3 is a graph of excitation and emission spectra of the near infrared phosphor obtained in the first set of baking experiments, which can obtain that the optimal emission wavelength of the phosphor is 780nm, the optimal excitation wavelength is 450nm, and the phosphor is very matched with a commercial blue light chip, and is suitable for preparing a near infrared LED device excited by blue light.
The obtained near infrared fluorescent powder and a blue light LED chip are packaged and fluorescence spectrum is tested, and the result shows that the emission peak of the fluorescent powder obtained by the first group of roasting experiments is between 650 and 1150nm, and the half-peak width is 149nm.
The emission peak of the fluorescent powder obtained by the second group of roasting experiments is between 650 and 1120nm, and the half-peak width is 153nm.
Fig. 4 is an emission spectrum of the near infrared fluorescent powder obtained in the first set of baking experiments and the LED device prepared by the commercial blue light chip under different current driving, which shows that the fluorescent powder and the commercial blue light chip can be successfully prepared into the near infrared LED device, and the luminous intensity is enhanced along with the increase of the current, so that the luminous performance of the near infrared LED device is proved to be good.
Example 2
Cr 3+ Garnet-structure-doped broadband near infrared fluorescent powder Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ The preparation was the same as in example 1, except that the powder was a green solid powder: weighing CaCO according to stoichiometric ratio 3 :0.070g，Y 2 O 3 :0.09032g，Al 2 O 3 :0.09043g，GeO 2 :0.07321g，Cr 2 O 3 0.0019g. The roasting experiment is heated to 1000 ℃ at a heating rate of 5 ℃/min, then heated to 1500 ℃ at a heating rate of 2 ℃/min, and then kept for 6 hours, and cooled to room temperature at a cooling rate of 2 ℃/min.
The obtained near infrared fluorescent powder is tested for fluorescence spectrum, and the result shows that the emission spectrum of the obtained fluorescent powder is between 650 and 1120nm, and the half-peak width is 148nm.
Example 3
Cr 3+ Garnet-structure-doped broadband near infrared fluorescent powder
Ca 2.35 Y 0.65 Al 1.95 Al 0.65 Ge 2.35 O 12 :0.05Cr 3+ The preparation was the same as in example 1, except that the powder was a green solid powder: weighing CaCO according to stoichiometric ratio 3 :0.1175g，Y 2 O 3 :0.03669g，Al 2 O 3 :0.06624g，GeO 2 :0.12289g，Cr 2 O 3 0.0019g. Calcination experiment at 5 °c-The temperature rising rate of min rises to 1000 ℃, then the temperature rises to 1450 ℃ at the temperature rising rate of 2 ℃/min, the temperature is kept for 6 hours, and then the temperature is reduced to room temperature at the temperature reducing rate of 2 ℃/min.
The obtained near infrared fluorescent powder is tested for fluorescence spectrum, and the result shows that the emission spectrum of the obtained fluorescent powder is between 650 and 1150nm, and the half-peak width is 153nm.
Example 4
Cr 3+ Broadband near infrared fluorescent powder doped with garnet structure
Ca 1.4 Y 1.6 Al 1.95 Al 1.6 Ge 1.4 O 12 :0.05Cr 3+ The preparation was the same as in example 1, except that the powder was a green solid powder: weighing CaCO according to stoichiometric ratio 3 :0.070g，Y 2 O 3 :0.09032g，Al 2 O 3 :0.09043g，GeO 2 :0.07321g，Cr 2 O 3 0.0019g. The roasting experiment is heated to 1000 ℃ at a heating rate of 5 ℃/min, then heated to 1450 ℃ at a heating rate of 2 ℃/min, and then kept for 6 hours, and cooled to room temperature at a cooling rate of 2 ℃/min.
The obtained near infrared fluorescent powder is tested for fluorescence spectrum, and the result shows that the emission spectrum of the obtained fluorescent powder is between 650 and 1150nm, and the half-peak width is 153nm.
Comparative example
Cr 3+ Garnet-structure-doped broadband near infrared fluorescent powder Ca 3 Al 1.95 Ge 3 O 12 :0.05Cr 3+ The preparation was the same as in example 1, except that the powder was a green solid powder: weighing CaCO according to stoichiometric ratio 3 :0.150g，Al 2 O 3 :0.04968g，GeO 2 :0.15689g，Cr 2 O 3 0.0019g. The roasting experiment is heated to 1000 ℃ at a heating rate of 5 ℃/min, then heated to 1450 ℃ at a heating rate of 2 ℃/min, and then kept for 6 hours, and cooled to room temperature at a cooling rate of 2 ℃/min.
The obtained near infrared fluorescent powder is subjected to fluorescence spectrum test, and the result shows that the emission peak of the obtained fluorescent powder is between 650 and 1000nm, and the half-peak width is 95nm.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (7)
1. Cr (chromium) 3+ The doped broadband near infrared fluorescent powder is characterized in that the chemical general formula of the fluorescent powder is A1 3- y A2 y B 2-x C1 y C2 3-y O 12 :xCr 3+ (0 < y < 3,0 < x.ltoreq.0.14), wherein a1= Ca, mg, ba, cd, sr, zn; a2 = Y, gd, la, in; b=c1= Al, ga, sc, lu; c2 = Ge, si, ti, hf, zr.
2. Cr according to claim 1 3+ The doped broadband near infrared fluorescent powder is characterized in that in the chemical general formula, B and C1 are the same elements and occupy octahedral sites and tetrahedral sites respectively, and the ionic radius of B and C1 is larger than C2; a1 and A2 occupy dodecahedral sites and have an ionic radius greater than B and C1.
3. Cr according to claim 2 3+ The doped broadband near infrared fluorescent powder is characterized in that the chemical expression of the fluorescent powder is Ca 2 Y 1 Al 1.95 Al 1 Ge 2 O 12 :0.05Cr 3+ The excitation peak is 450nm, the emission peak is 780nm, and the full width at half maximum is 149nm.
4. A Cr as claimed in any one of claims 1 to 3 3+ The preparation method of the doped broadband near infrared fluorescent powder adopts a high-temperature solid phase sintering method, and is characterized by comprising the following specific steps:
(a) Weighing the corresponding oxides or carbonates of A1, A2, B, C1 and C2 according to the molecular formula of the fluorescent powder, fully mixing, adding a certain amount of fluxing agent, and grinding uniformly;
(b) Loading the mixture obtained in the step (a) into a corundum crucible or a graphite crucible, transferring the corundum crucible or the graphite crucible into a tube furnace, sintering at a certain temperature, preserving heat for a period of time, and then cooling to room temperature;
(c) Fully grinding the sintered product obtained in the step (b) to obtain a novel Cr 3+ A broadband near infrared fluorescent powder doped with garnet structure.
In step (a), the fluxing agent is B 2 O 3 、Li 2 CO 3 、CaF 2 、P 2 O 5 、LiF、NH 4 F、K 2 CO 3 One or more of the following; the added content is 1-7wt% of the total mass of the fluorescent powder synthetic raw material.
5. Cr according to claim 4 3+ The preparation method of the doped broadband near infrared fluorescent powder is characterized in that in the step (b), the sintering times are one or more times.
6. Cr according to claim 5 3+ The preparation method of the doped broadband near infrared fluorescent powder is characterized in that in the step (b), the heating rate is 3-10 ℃/min, the roasting temperature is 700-1600 ℃, and the single roasting time is 3-8 h.
7. A Cr as claimed in any one of claims 1 to 3 3+ Use of doped broadband near infrared phosphor in near infrared LED light source, characterized in that the Cr 3+ The doped broadband near infrared fluorescent powder is applied to a near infrared LED light source, the excitation peak is 450nm, the emission spectrum is 650-1150 nm, and the half-peak width is 95-153 nm.
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