CN116425547B - Chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and preparation method thereof - Google Patents
Chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910001430 chromium ion Inorganic materials 0.000 title claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 11
- 150000003325 scandium Chemical class 0.000 title claims abstract description 11
- 239000011651 chromium Substances 0.000 claims abstract description 46
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 34
- 239000000843 powder Substances 0.000 abstract description 25
- 239000000126 substance Substances 0.000 abstract description 9
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- 229910052804 chromium Inorganic materials 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 230000003213 activating effect Effects 0.000 description 6
- 238000000695 excitation spectrum Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 3
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000006862 quantum yield reaction Methods 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/553—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on fluorides
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C09K11/7704—Halogenides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
- C04B2235/445—Fluoride containing anions, e.g. fluosilicate
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/9646—Optical properties
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses a chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and a preparation method thereof, wherein the chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material is obtained by a hydrothermal method and high-temperature hot-press post-treatment, and has the chemical formula: k (K) 2 LiSc 1‑x Cr x F 6 X=0.10 to 0.20. The material has a strong broadband absorption peak between 350 and 500 nanometers, can be excited by a blue light chip, has a strong broadband emission peak around 770 nanometers, and has higher density compared with the corresponding powder material, thereby having better heat conductivity and thermal stability, and can be used for packaging high-power NIRpc-LED devices.
Description
Technical field:
the invention relates to the technical field of inorganic luminescent materials, in particular to a chromium ion activated scandium-based fluoride broadband near infrared luminescent material and a preparation method thereof.
The background technology is as follows:
near infrared spectrum detection technology is widely applied to daily life and industrial production, and near infrared fluorescence conversion type light emitting diode (NIR pc-LED) is attracting attention in recent years as a next-generation intelligent near infrared light source. Near infrared luminescent materials are one of the key components of NIRpc-LEDs and play a vital role in the performance of NIRpc-LED devices.
Among the numerous transition metal ions, cr 3+ The blue light broadband absorption (which can be excited by an InGaN blue light chip) and near infrared broadband emission are strong; in addition, due to Cr 3+ Unique 3d 3 The electron configuration, the position and the peak width of the emission peak of the broadband near infrared luminescent material can be easily adjusted by changing the crystal field, and the special properties completely meet the requirements of the near infrared luminescent material for NIR pc-LED, so that people can know Cr 3+ Ion activated broadband proximityInfrared light emitting materials have been intensively studied.
The invention comprises the following steps:
the invention aims to provide a chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material and a preparation method thereof, wherein the chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material is prepared by a hydrothermal method and high-temperature hot-pressing post-treatment, has a very strong broadband absorption peak between 350 and 500 nanometers, can be excited by a blue light chip, has a very strong broadband emission peak around 770 nanometers, and has higher density compared with a corresponding powder material, so that the ceramic material has better thermal conductivity and thermal stability, and can be used for packaging high-power NIRpc-LED devices.
The invention is realized by the following technical scheme:
a chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material has a chemical formula: k (K) 2 LiSc 1- x Cr x F 6 ，x＝0.10～0.20。
The preparation method of the material comprises the following steps: will (NH) 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF (1-x) in a molar ratio of (7-12) into deionized water, stirring, transferring the solution into a hydrothermal reaction kettle, preserving heat at 200 ℃ for 10 hours, naturally cooling to room temperature, centrifuging to obtain precipitate, washing with deionized water, washing with absolute ethyl alcohol, drying at 75 ℃ for 3 hours, and then treating at 600 ℃ for 5 hours under 220Mpa to obtain a final product K 2 LiSc 1-x Cr x F 6 Broadband near infrared luminescent ceramic material.
Pure phases are obtained only in the presence of an excess of KF, and (NH) 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 O and KF are optimal in luminous intensity at the ratio of (1-x): x:1:10.
The invention also protects application of the chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material for packaging high-performance NIRpc-LED devices.
Advantageous effects of the inventionThe effects are as follows: the chromium ion activated fluoride broadband near infrared luminescent ceramic material prepared by the hydrothermal method and the high-temperature hot-pressing post-treatment has a strong broadband absorption peak between 350 and 500 nanometers, can be excited by a blue light chip, has a strong broadband emission peak around 770 nanometers, and is treated for 5 hours at 600 ℃ and 220Mpa to obtain the ceramic material with the density obviously higher than that of a corresponding powder material, so that the ceramic material has better thermal conductivity and thermal stability and can be used for packaging high-performance NIR pc-LED devices. The quantum efficiency of the prepared near infrared luminescent ceramic material is higher than that of the reported K 2 NaScF 6 :Cr 3+ (Laser&Photonics Reviews,2020,15,2000410) and K 2 NaInF 6 :Cr 3+ Near infrared luminescent powder material (Chemical Engineering Journal,2022,427,131740).
Description of the drawings:
FIG. 1 is a Cr produced in example 1 3+ Activating the fluorescence excitation spectrum of the broadband near infrared luminescent ceramic material.
FIG. 2 is a Cr produced in example 2 3+ Activating the fluorescence excitation spectrum of the broadband near infrared luminescent ceramic material.
FIG. 3 is a Cr produced in example 3 3+ Activating the fluorescence excitation spectrum of the broadband near infrared luminescent ceramic material. As can be seen from FIG. 3, the product has a strong broadband absorption peak between 350 and 500 nm, which can be excited by the blue light chip.
FIG. 4 is a fluorescence excitation spectrum of the Cr3+ activated broadband near infrared luminescent ceramic material prepared in example 4.
FIG. 5 is a fluorescence excitation spectrum of the Cr3+ activated broadband near infrared luminescent ceramic material prepared in example 5.
FIG. 6 is a fluorescence excitation spectrum of the Cr3+ activated broadband near infrared luminescent ceramic material prepared in example 6.
FIG. 7 is a drawing of Cr produced in example 3 3+ Activating the fluorescence emission spectrum of the broadband near infrared luminescent ceramic material. As can be seen from FIG. 7, the product has very strong broadband near infrared emission around 770 nm, and can be used for packaging high-performance NIRpc-LED devices.
FIG. 8 is a graph showing the comparison of the luminous intensity of the products obtained in examples 1 to 4. As can be seen from FIG. 8, when KF: li (OH). H 2 The luminous intensity of the material is strongest when the molar ratio of O is 10:1.
FIG. 9 is example 3 and reported K 2 NaScF 6 :Cr 3+ 、K 2 NaInF 6 :Cr 3+ Quantum yield contrast plot for near infrared luminescent powder materials. As can be seen from FIG. 9, this patent K 2 LiScF 6 :Cr 3+ The quantum yield of the ceramic material is superior to that of the reported K 2 NaScF 6 :Cr 3+ And K 2 NaInF 6 :Cr 3+ Near infrared luminescent powder material.
FIG. 10 is a drawing showing the Cr produced in comparative example 1 3+ And activating the broadband near infrared luminous powder scanning electron microscope picture. As can be seen from fig. 10, the powder material is in the form of dispersed spheres, and the particles are relatively dispersed.
FIG. 11 is a drawing of Cr produced in example 3 3+ And activating the scanning electron microscope picture of the broadband near infrared luminescent ceramic material. Compared with the powder material in fig. 10, the ceramic material in fig. 11 has obviously higher compactness, so that the ceramic material can have better heat conductivity and thermal stability than the powder material, and can be used for high-power NIRpc-LED devices.
The specific embodiment is as follows:
the following is a further illustration of the invention and is not a limitation of the invention.
Example 1:
cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.90 Cr 0.10 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.90:0.10:1:6 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml deionized water, stirring for 10 min, transferring the solution into a hydrothermal reaction kettle, preserving heat at 200 ℃ for 10 h, naturally cooling to room temperature, centrifuging the solution to obtain precipitateWashing with deionized water for 3 times, then washing with ethanol for 3 times, and drying at 75 ℃ for 3 hours to obtain the broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and the final product broadband near infrared luminescent ceramic material is obtained after natural cooling to room temperature.
Example 2
Cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.90 Cr 0.10 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.90:0.10:1:8 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml of deionized water, stirring for 10 minutes, transferring the solution into a hydrothermal reaction kettle, preserving heat for 10 hours at 200 ℃, naturally cooling to room temperature, centrifuging the solution obtained in the steps to obtain precipitate, washing 3 times with deionized water, washing 3 times with ethanol, and drying for 3 hours at 75 ℃ to obtain the broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and the final product broadband near infrared luminescent ceramic material is obtained after natural cooling to room temperature.
Example 3
Cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.90 Cr 0.10 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.90:0.10:1:10 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml deionized water, stirring for 10 min, transferring the solution into a hydrothermal reaction kettle, preserving heat at 200 ℃ for 10 h, naturally cooling to room temperature, centrifuging the solution obtained in the above step to obtain precipitate, washing with deionized water for 3 times, and then washing with ethyl acetateWashing with alcohol for 3 times, and drying at 75deg.C for 3 hours to obtain broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and the final product broadband near infrared luminescent ceramic material is obtained after natural cooling to room temperature.
Comparative example 1
Cr (chromium) 3+ Doped broadband near infrared luminescent powder material with chemical formula of K 2 LiSc 0.90 Cr 0.10 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent powder material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.90:0.10:1:10 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml of deionized water, stirring for 10 minutes, transferring the solution into a hydrothermal reaction kettle, preserving heat for 10 hours at 200 ℃, naturally cooling to room temperature, centrifuging the solution obtained in the steps to obtain precipitate, washing 3 times with deionized water, washing 3 times with ethanol, and drying for 3 hours at 75 ℃ to obtain the broadband near infrared luminescent powder material.
Example 4
Cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.90 Cr 0.10 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.90:0.10:1:12 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml of deionized water, stirring for 10 minutes, transferring the solution into a hydrothermal reaction kettle, preserving heat for 10 hours at 200 ℃, naturally cooling to room temperature, centrifuging the solution obtained in the steps to obtain precipitate, washing 3 times with deionized water, washing 3 times with ethanol, and drying for 3 hours at 75 ℃ to obtain the broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and naturally cooled to room temperature to obtain the final productThe material is a broadband near infrared luminescent ceramic material.
Example 5
Cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.85 Cr 0.15 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.85:0.15:1:10 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml of deionized water, stirring for 10 minutes, transferring the solution into a hydrothermal reaction kettle, preserving heat for 10 hours at 200 ℃, naturally cooling to room temperature, centrifuging the solution obtained in the steps to obtain precipitate, washing 3 times with deionized water, washing 3 times with ethanol, and drying for 3 hours at 75 ℃ to obtain the broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and the final product broadband near infrared luminescent ceramic material is obtained after natural cooling to room temperature.
Example 6
Cr (chromium) 3+ Doped broadband near infrared luminescent ceramic material with chemical formula of K 2 LiSc 0.80 Cr 0.20 F 6 。
Cr described above 3+ The preparation method of the doped broadband near infrared luminescent ceramic material comprises the following steps:
at room temperature, weighing (NH) according to the molar ratio of 0.80:0.20:1:10 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF into 25 ml of deionized water, stirring for 10 minutes, transferring the solution into a hydrothermal reaction kettle, preserving heat for 10 hours at 200 ℃, naturally cooling to room temperature, centrifuging the solution obtained in the steps to obtain precipitate, washing 3 times with deionized water, washing 3 times with ethanol, and drying for 3 hours at 75 ℃ to obtain the broadband near infrared luminescent powder material. The powder material is further kept at 600 ℃ and 220Mpa for 5 hours, and the final product broadband near infrared luminescent ceramic material is obtained after natural cooling to room temperature.
Claims (3)
1. The preparation method of the chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material is characterized by comprising the following steps of: will (NH) 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 Adding O and KF (1-x) in a molar ratio of (7-12) into deionized water, stirring, transferring the solution into a hydrothermal reaction kettle, preserving heat at 200 ℃ for 10 hours, naturally cooling to room temperature, centrifuging to obtain precipitate, washing with deionized water, washing with absolute ethyl alcohol, drying at 75 ℃ for 3 hours, and then treating at 600 ℃ for 5 hours under 220Mpa to obtain a final product K 2 LiSc 1-x Cr x F 6 Broad band near infrared luminescent ceramic material, x=0.10-0.20.
2. The method according to claim 1, wherein (NH) 4 ScF 6 、(NH) 4 CrF 6 、Li(OH)·H 2 The molar ratio of O to KF is (1-x): x:1:10.
3. The application of the chromium ion activated scandium-based fluoride broadband near infrared luminescent ceramic material obtained by the preparation method of claim 1, which is characterized by being used for packaging high-performance NIRpc-LED devices.
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