CN117363350A - Tantalate near-infrared fluorescent material and preparation method thereof - Google Patents
Tantalate near-infrared fluorescent material and preparation method thereof Download PDFInfo
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- CN117363350A CN117363350A CN202311379315.7A CN202311379315A CN117363350A CN 117363350 A CN117363350 A CN 117363350A CN 202311379315 A CN202311379315 A CN 202311379315A CN 117363350 A CN117363350 A CN 117363350A
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- 239000000463 material Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 5
- 230000000630 rising effect Effects 0.000 claims 1
- 238000005424 photoluminescence Methods 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 description 15
- 229910044991 metal oxide Inorganic materials 0.000 description 15
- 150000004706 metal oxides Chemical class 0.000 description 15
- 229910052593 corundum Inorganic materials 0.000 description 12
- 239000010431 corundum Substances 0.000 description 12
- 238000001035 drying Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 230000005284 excitation Effects 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000004570 mortar (masonry) Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000000103 photoluminescence spectrum Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention discloses a tantalate near-infrared fluorescent material and a preparation method thereof, and belongs to the technical field of near-infrared photoluminescence fluorescence. The tantalate near-infrared fluorescent material is prepared by adopting a solid phase method, and the chemical formula of the tantalate near-infrared fluorescent material is Ga 1‑x TaO 4 :xNi 2+ Wherein x is more than 0 and less than or equal to 0.01. The invention is prepared by doping GaTaO with Ni 4 Obtaining Ga 1‑ x TaO 4 :xNi 2+ Can emit near infrared light of 1541nm-1566nm, has high luminous efficiency and long luminous life, can be matched with a commercial purple light chip to emit purple light with the emission center near 428nm, emits near infrared light of about 1541nm-1566nm, and has wide application prospect in the fields of lighting and display lamplight and electricity.
Description
Technical Field
The invention belongs to the technical field of near infrared photoluminescence fluorescence, and particularly relates to a tantalate near infrared fluorescent material and a preparation method thereof.
Background
Metal oxides have significant advantages as a new generation of luminescent materials in the following respects: (1) high-efficiency luminescence: the metal oxides can emit light by exciting electron transitions, and their internal energy level structure and electron band structure enable them to produce a highly efficient light emitting effect. This makes the metal oxide a very bright and efficient luminescent material. (2) High stability: metal oxides generally have high stability under high temperature and humidity conditions. The luminescence properties of metal oxides are less likely to decay over long periods of use and in harsh environments compared to other luminescent materials. This allows for a longer service life of the metal oxide in various applications. (3) Broad light emission spectral range: the metal oxide can realize luminescence in a wide band by adjusting its chemical composition and crystal structure. This allows the metal oxide to emit light at multiple wavelengths, from ultraviolet to visible and infrared. This property makes metal oxides have a wide range of application potential in different fields. (4) Regulatability: the luminescence properties of the metal oxide can be tailored by adjusting its composition, crystal structure and impurity doping. This means that the metal oxide material can be designed and synthesized according to specific requirements to achieve desired luminescence properties such as luminescence intensity, wavelength, luminescence time, etc. (5) Rich application fields: metal oxides have a wide range of application potential. They can be used in lighting and display technologies such as Light Emitting Diodes (LEDs) and Organic Light Emitting Diodes (OLEDs), as well as in the fields of bioimaging, sensors, photovoltaic devices, etc. The luminescent properties of metal oxides make them of great application prospect in many different fields.
Therefore, the metal oxide as a new generation luminescent material has the advantages of high-efficiency luminescence, high stability, wide luminescence spectrum range, adjustability, wide application field and the like, so that the metal oxide becomes an ideal choice for various photoelectrons and optical applications.
However, the existing tantalate structural materials still have some defects, including lower luminous efficiency, higher cost, short luminous life, emission peak wavelength concentrated within 800nm, and narrow half-width of near infrared emission.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a tantalate near-infrared fluorescent material and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
tantalate near-infrared fluorescent material with chemical formulaIs Ga 1-x TaO 4 :xNi 2+ Wherein x is more than 0 and less than or equal to 0.01.
As a preferred embodiment of the invention, the tantalate near-infrared fluorescent material generates near-infrared light with the emission peak of which the luminescence center is located at 1541nm-1566nm under the excitation of light with the wavelength of 428 nm.
More preferably, the tantalate near-infrared fluorescent material generates near-infrared light with an emission peak having a light emission center at 1566nm when excited by light with a wavelength of 428 nm.
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Ga is added 2 O 3 、Ta 2 O 5 Mixing NiO raw materials, adding absolute ethyl alcohol, and grinding;
(2) And then calcining and cooling to obtain the tantalate near infrared fluorescent material.
As a preferred embodiment of the invention, the temperature rise rate of the calcination is 5 ℃/min, the calcination temperature is 1300-1500 ℃ and the time is 1-5h.
As a preferred embodiment of the present invention, the volume ratio of the total mass of the raw material mixture to the absolute ethanol is 1g: (4-7) ml.
As a preferred embodiment of the present invention, the milling time is 20 to 60 minutes.
As a preferred embodiment of the present invention, the calcined atmosphere is at least one of air, nitrogen and argon.
As a preferred embodiment of the present invention, the Ga 2 O 3 、Ta 2 O 5 The purity of the NiO raw material is 99.99 percent.
Compared with the prior art, the invention has the beneficial effects that: the invention is prepared by doping GaTaO with Ni 4 Obtaining Ga 1-x TaO 4 :xNi 2+ Wherein Ni replaces gallium to cause lattice expansion, and the change of the material structure causes red shift of luminescence peak, so that the material emits near infrared light of 1541nm-1566nm under the excitation wavelength of 428nm, and has high luminescence intensity and long luminescence life.
Drawings
Fig. 1 is an XRD pattern of the tantalate near infrared fluorescent material prepared in example 1.
FIG. 2 is a photoluminescence chart of the tantalate near infrared fluorescent material prepared in example 1 at room temperature under excitation of a xenon lamp with a wavelength of 428nm as a light source.
FIG. 3 is a graph showing the excitation spectrum of the tantalate near infrared fluorescent material prepared in example 1.
FIG. 4 is a graph showing the comparison of the relative luminous intensity of the tantalate near infrared fluorescent material prepared in examples 1-3.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Will be 24.9mmolGa 2 O 3 、25mmolTa 2 O 5 Mixing 0.2 mmole of NiO raw materials, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol into the agate mortar, and grinding the agate mortar for 30 minutes; the volume ratio of the total mixed mass of the raw materials to the absolute ethyl alcohol is 1g to 4ml.
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1500 ℃ for 4 hours, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
As can be seen from FIG. 1, example 1 successfully produced tantalate near-infrared fluorescent material Ga with good crystallinity 1-x TaO 4 :xNi 2 + 。
As can be seen from FIG. 2, under 428nm light excitation, the photoluminescence spectrum of the prepared tantalate near infrared fluorescent material is broadband near infrared light with an emission center at 1542nm, the half-width of the broadband near infrared light reaches 1542nm, and the relative luminous intensity is shown in FIG. 4.
As can be seen from FIG. 3, the prepared tantalate near infrared fluorescent material has two excitation spectraPeaks at 272nm and 428nm, respectively, which correspond to Ni 2+ Is a broadband near infrared characteristic excitation peak of (c).
Example 2
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Will be 24.95mmolGa 2 O 3 、25mmolTa 2 O 5 Mixing 0.1 mmole of NiO raw material, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol, and grinding for 20min; the volume ratio of the total mixed mass of the raw materials to the absolute ethyl alcohol is 1g to 6ml.
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1300 ℃ for 5 hours, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
The tantalate near infrared fluorescent material prepared in example 2 has a photoluminescence spectrum of broadband near infrared light with an emission center at 1541nm under 428nm light excitation, and the relative luminescence intensity is shown in fig. 4.
Example 3
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Will be 24.75mmolGa 2 O 3 、25mmolTa 2 O 5 Mixing 0.5 mmole of NiO raw materials, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol, and grinding for 60 minutes; the volume ratio of the total mixed mass of the raw materials to the absolute ethyl alcohol is 1 g/7 ml.
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1500 ℃ for 1h, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
The tantalate near infrared fluorescent material prepared in example 3 has a photoluminescence spectrum of broadband near infrared light with an emission center at 1566nm under 428nm light excitation, and the relative luminous intensity is shown in fig. 4.
Comparative example 1
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) 25mmolGa 2 O 3 、25mmolTa 2 O 5 After the raw materials are mixed, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol, and grinding for 30min;
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1500 ℃ for 4 hours, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
The tantalate near-infrared fluorescent material prepared in comparative example 1 has no luminescence phenomenon under 428nm light excitation.
Comparative example 2
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Will be 24mmolGa 2 O 3 、25mmolTa 2 O 5 Mixing 2mmolNiO raw materials, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol, and grinding for 30min;
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1500 ℃ for 4 hours, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
The tantalate near-infrared fluorescent material prepared in comparative example 2 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 1572nm under 428nm light excitation; comparative example 2 significantly reduced the luminescence intensity of the material due to concentration quenching compared to examples 1-4.
Comparative example 3
A preparation method of a tantalate near-infrared fluorescent material comprises the following steps:
(1) Will be 24.9mmolGa 2 O 3 、25mmolTa 2 O 5 、0.2mmolCr 2 O 3 After the raw materials are mixed, placing the mixed powder into an agate mortar, dripping a proper amount of absolute ethyl alcohol, and grinding for 20min; the volume ratio of the total mixed mass of the raw materials to the absolute ethyl alcohol is 1g to 6ml.
(2) And (3) putting the ground powder into a drying oven at 70 ℃ for drying for half an hour, taking out, continuously grinding until the material is in a powder state, transferring the material into a corundum crucible, placing the corundum crucible into a tube furnace, heating at a speed of 5 ℃/min, sintering at 1300 ℃ for 5 hours, and finally naturally cooling to room temperature to obtain the tantalate near infrared fluorescent material.
The tantalate near-infrared fluorescent material prepared in comparative example 3 has a photoluminescence spectrum of broadband near-infrared light with an emission center at 827nm under 428nm light excitation. Compared with the material of comparative example 3, the tantalate near-infrared fluorescent material prepared in examples 1-3 has wider half-width of the luminescence peak, comprises a near-infrared two region and a near-infrared three region, and has important effects on the aspects of treating cancers, tumor cells and the like.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. A tantalate near-infrared fluorescent material is characterized by having a chemical formula of Ga 1-x TaO 4 :xNi 2+ Wherein x is more than 0 and less than or equal to 0.01.
2. The tantalate near-infrared fluorescent material of claim 1 wherein the tantalate near-infrared fluorescent material produces near-infrared light having an emission peak with a luminescence center at 1541nm-1566nm when excited by light having a wavelength of 428 nm.
3. The method for preparing the tantalate near-infrared fluorescent material according to claim 1 or 2, characterized by comprising the following steps:
(1) Ga is added 2 O 3 、Ta 2 O 5 Mixing NiO raw materials according to stoichiometric ratio, adding absolute ethyl alcohol, and grinding;
(2) And then calcining and cooling to obtain the tantalate near infrared fluorescent material.
4. The method for preparing the near infrared fluorescent material of optical tantalate according to claim 3, wherein the temperature rising rate of the calcination is 5 ℃/min, the calcination temperature is 1300-1500 ℃ and the time is 1-5h.
5. The method for preparing the near infrared fluorescent material of optical tantalate according to claim 3, wherein the volume ratio of the total mixed mass of the raw materials to absolute ethyl alcohol is 1g: (4-7) ml.
6. The method for preparing a near infrared fluorescent material of claim 3, wherein the calcined atmosphere is at least one of air, nitrogen and argon.
7. The method for preparing a near infrared fluorescent material of claim 3, wherein said Ga 2 O 3 、Ta 2 O 5 The purity of the NiO raw material is 99.99 percent.
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| CN202311379315.7A CN117363350A (en) | 2023-10-24 | 2023-10-24 | Tantalate near-infrared fluorescent material and preparation method thereof |
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| CN202311379315.7A CN117363350A (en) | 2023-10-24 | 2023-10-24 | Tantalate near-infrared fluorescent material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110054793A (en) * | 2009-11-18 | 2011-05-25 | 중앙대학교 산학협력단 | Preparation method for cathode fluorescent body of lamp |
| US20140112876A1 (en) * | 2011-03-23 | 2014-04-24 | Ihi Corporation | Ultraviolet light absorber and cosmetic material using the same |
| CN105378030A (en) * | 2013-05-02 | 2016-03-02 | 默克专利股份有限公司 | Phosphors |
| CN113481006A (en) * | 2021-07-14 | 2021-10-08 | 广东工业大学 | Near-infrared broad-spectrum fluorescent material and preparation method and application thereof |
-
2023
- 2023-10-24 CN CN202311379315.7A patent/CN117363350A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110054793A (en) * | 2009-11-18 | 2011-05-25 | 중앙대학교 산학협력단 | Preparation method for cathode fluorescent body of lamp |
| US20140112876A1 (en) * | 2011-03-23 | 2014-04-24 | Ihi Corporation | Ultraviolet light absorber and cosmetic material using the same |
| CN105378030A (en) * | 2013-05-02 | 2016-03-02 | 默克专利股份有限公司 | Phosphors |
| CN113481006A (en) * | 2021-07-14 | 2021-10-08 | 广东工业大学 | Near-infrared broad-spectrum fluorescent material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| ANDREW C. MALINGOWSKI等: "Substitutional Mechanism of Ni into the Wide-Band-Gap Semiconductor InTaO4 and Its Implications for Water Splitting Activity in the Wolframite Structure Type", 《INORGANIC CHEMISTRY》, vol. 51, 24 April 2012 (2012-04-24), pages 6096 * |
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