CN115717073A - Broadband near-infrared luminescent material and preparation method and application thereof - Google Patents
Broadband near-infrared luminescent material and preparation method and application thereof Download PDFInfo
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- 238000000034 method Methods 0.000 claims abstract description 14
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The invention discloses a near-infrared broadband luminescent material and a preparation method and application thereof. The general formula of the chemical component of the fluorescent luminescent material is A 2 Mg 1‑x TiO 6 ：Ni 2+ Wherein A is Y or Gd, and x is more than or equal to 0.01 and less than or equal to 0.08. The raw materials are weighed according to the stoichiometric ratio corresponding to the general formula of the chemical components, mixed and stirred, and the high-temperature solid phase method is adopted for preparation, so that the process is simple, the production cost is low, and the chemical properties of the product are stable. The material obtained by the invention can show broadband infrared luminescence within the range of 1100-1700nm, and the method has the advantages of low cost, easily obtained raw materials, environment-friendly production process and no waste gas and waste liquid discharge.
Description
Technical Field
The invention relates to a luminescent material, in particular to a broadband near-infrared luminescent material, a preparation method and application thereof.
Background
Near Infrared (NIR) region is a small portion of electromagnetic waves with a wavelength range of 780-2526 nm, and due to its invisible property and strong penetration ability, near infrared light sources are receiving more and more attention, and have very wide applications in the fields from near infrared spectroscopy to optical communication, night vision, photodynamic therapy, biomedical imaging, and the like. The emission of the recently reported near infrared light sources is mainly limited to the short-wave near infrared region of less than 1000 nm. However, according to Rayleigh scattering, near infrared two-region (NIR-II, 1000-1700 nm) light is superior to near infrared one-region (NIR-I, 700-1000 nm) light due to a lower optical scattering coefficient. Compared with the near infrared first region (NIR-I, 700-1000 nm), the near infrared second region fluorescence has the advantages of low scattering in organisms, deep tissue penetration and high imaging resolution, so that the near infrared second region fluorescence becomes a technology with great development potential. In this regard, a wider range of near infrared light is needed as a support for quantitative analysis and diagnostic techniques for near infrared light sources to obtain comprehensive chemical and physical information. The existing near infrared light sources on the market at present have two kinds, one of which is a heat light source comprising a tungsten/halogen lamp and a globe lamp, and although the heat light source has ultra-wide bandwidth, the defects of large volume, high power consumption, limited service life, serious heat dissipation and the like are inevitable. Another is a non-thermal light source like lasers and light emitting diodes, which also affects its application due to extremely narrow bandwidth and spectral instability. Therefore, the research on novel near-infrared luminescent materials covering 1100-1700nm wave bands is of great significance.
The rare earth ion luminescence comes from 4f-4f electron layer transition, and the luminescent bandwidth is greatly limited due to outermost electron shielding, so that the requirement of ultra-wideband luminescence cannot be met. The transition metal ion luminescence comes from 3d electron layer transition, is obviously influenced by a surrounding coordination field, and can realize broadband luminescence of a near-infrared band. The transition metal elements capable of emitting light in a broadband of 1000-1700nm in an optical communication waveband are mainly concentrated in Cr 4+ 、Ni 2+ 、Mn 6+ 、V 2+ Medium, however, cr 4+ 、Mn 6+ 、V 2+ Valence state instability in the material, and valence state regulation is required to obtain the expected infrared active center, so that the application of the material in a gain material is greatly limited.
Due to transition metal ions Ni 2+ Special electron shell structure of (2) so that Ni 2+ The ion generally has controllability in the light emission in an octahedral hexa-coordinated environment and broadband absorption and emission characteristics in the near infrared region. At the same time Ni 2+ Has stable valence state, does not need special atmosphere control, and is compared with other transition metal elements, ni 2+ The fluorescent material has obvious advantages as a near-infrared luminescence center. With respect to Ni 2+ The study make internal disorder or usurp of ion near-infrared broadband luminescence dates back to 60 s in the last century at first, and MgGa was observed at room temperature by Takenobu Suzuki et al 2 O 4 ：Ni 2+ The spinel is in the range of 1100-1600 nmThere is a wide emission band (Journal of luminescences 113 (2005) 265-270). Both C.Matuszewska and L.Marciniak in (Sr, ca, ba, mg) TiO 3 ：Ni 2+ The broadband luminescence of 1100nm-1600nm is realized, and Ni is different from the substrate 2+ The emission peak of the ion is shifted by about 500nm (Journal of Luminescence 223 (2020) 117221). Broad-band NIR emission with a center wavelength of 1430nm and a full width at half maximum (FWHM) of 230nm is reported by Guinliang Yu et al in a Ni2+ ion doped perovskite NaSbO3 lattice (Ceramics International 47 (2021) 776-781). Cuiping Wang et al doping Zn in nickel 1+y Sn y Ga 2-2y O 4 In solid solution, the broadband luminescence of 1100nm-1600nm (J.Mater.chem.C, 2021,9,4583-4590) is realized. Feng Liu et al in Zn 3 Ga 2 Ge 2 O 10 :Ni 2+ The ultra-wide light emission of 1050-1600nm is realized (adv. Optical mater.2016,4, 562-566). Garnet solid solution Y in Lifang Yuan et al 3 Al 2 Ga 3 O 12 The broadband light emission is realized, the emission center is located at 1450nm, and the maximum half-height width is 300nm (ACS appl. Mater. Interfaces2022,14, 4265-4275). Martins a Et al in BaLiF 3 :Ni 2+ The ultra-wide light emission of 1100nm to 2000nm is realized (Journal of Luminescence 62 (1994) 281 to 289).
In view of the research situation of the nickel-doped near-infrared luminescent phosphor, most of the nickel-doped near-infrared luminescent phosphor uses germanate or gallate as a matrix material, but the germanate or gallate is expensive, and the titanate has low cost and is easy to obtain. Secondly, the nickel-doped near-infrared luminescent fluorescent powder synthesized based on various fluorides has wider luminescent bandwidth, but the product can cause environmental pollution in the production and use processes. The invention is based on (Y, gd) 2 MgTiO 6 The near-infrared luminescent material with the nickel-doped matrix increases the variety of the broadband near-infrared luminescent fluorescent powder. Based on (Y, gd) 2 MgTiO 6 Doping with Ni 2+ The ionic near-infrared fluorescent powder can be effectively excited by light sources with various wave bands. In comparison, the material realizes the broadband covering the near infrared band of 1100-1700nm by luminescence, and has the advantages of low cost, easily obtained raw materials,simple process, environment-friendly production process, no waste gas and liquid discharge and the like.
Disclosure of Invention
Aiming at the problems that the existing germanate or gallate is high in price, fluoride pollutes the environment and the like, the fluorescent powder which is low in price, free of pollution to the environment and good in broadband near-infrared luminescence characteristic is developed and is important. The broadband near-infrared luminescent fluorescent powder material provided by the invention has stable chemical properties, and the absorption band of the material covers a plurality of wave bands, so that the material can be effectively excited by light sources of the wave bands. Meanwhile, the broadband light emission covering the near infrared band of 1100-1700nm can be realized, and the maximum full width at half maximum of the emission band is 270nm. The method also has the advantages of low cost, easily obtained raw materials, simple process, environment-friendly production process, no waste gas and waste liquid discharge and the like. The invention also aims to provide a preparation method of the broadband near-infrared luminescent phosphor.
The technical scheme of the invention is as follows:
a broadband near-infrared luminescent material is prepared from A 2 Mg 1-x TiO 6 Is a matrix, wherein A is Y or Gd, i.e. in a double perovskite structure (Y, gd) 2 MgTiO 6 As a matrix, reuse of transition metal Ni 2+ The ions show broadband near-infrared luminescence in the octahedral hexa-coordination environment of the matrix, and the chemical composition general formula of the obtained material is A 2 Mg 1-x TiO 6 ：xNi 2+ Wherein x is more than or equal to 0.01 and less than or equal to 0.08.
The preparation method of the broadband near-infrared luminescent material comprises the following steps:
(1) Weighing: according to the chemical component general formula A 2 Mg 1-x TiO 6 ：xNi 2+ Wherein A is Y and Gd, x is more than or equal to 0.01 and less than or equal to 0.08, and raw material yttrium oxide (Y) is weighed according to the corresponding stoichiometric ratio in the formula 2 O 3 ) Gadolinium oxide (Gd) 2 O 3 ) Magnesium oxide (MgO), titanium dioxide (TiO) 2 ) And nickel oxide (NiO);
(2) Mixing materials: uniformly mixing the weighed raw materials, and grinding to obtain a mixture;
(3) And (3) calcining: calcining the mixture obtained in the step (2);
(4) Naturally cooling, discharging and crushing to obtain the broadband near-infrared luminescent material.
Further, in the step (2), the milling time is 0.5 to 3 hours, preferably 1 to 2 hours.
Further, in the step (3), the calcination temperature is 1200 to 1600 ℃, preferably 1300 to 1500 ℃, more preferably 1400 to 1500 ℃.
The obtained broadband near-infrared luminescent material has absorption band covering multiple wide wave bands, and can be effectively excited by various light sources within the ranges of 300-500nm, 600-800nm and 900-1500 nm. Obviously, the excitation requirements of various common light sources such as an LED blue light source, an LED near-infrared light source and the like can be met. The luminescent powder can realize broadband luminescence covering near-infrared wave band 1100-1700nm, has maximum full width at half maximum of emission band of 270nm, and is especially suitable for being made into broadband near-infrared luminescent light sources.
Compared with the prior art, the invention has the following beneficial effects:
(1) The broadband near-infrared luminescent fluorescent powder material provided by the invention has ultra-wide emission of 1100nm-1700nm, and the maximum full width at half maximum is about 270nm.
(2) The invention is Ni 2+ The ion broadband near-infrared luminescent material provides a new matrix and can provide a new Ni 2+ A preparation method of doped broadband near-infrared fluorescent powder.
(3) The luminescent phosphor material is prepared by a high-temperature solid-phase reaction method, so that the cost is low, the raw materials are easy to obtain, the process is simple, the production process is environment-friendly, and no waste gas or waste liquid is discharged.
Drawings
FIG. 1 shows Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The absorption spectrum of the fluorescent powder under 400nm-1650 nm.
FIG. 2 shows Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The near infrared emission spectrum of a sample under 455nm laser excitation has two different emission peaks of 1348nm and 1420nm respectively, and the full width at half maximum of an emission band is 260nm.
FIG. 3 shows Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The near infrared emission spectrum of a sample under the excitation of 980nm laser has two different emission peaks of 1346nm and 1408nm respectively, and the full width at half maximum of an emission band is 230nm.
FIG. 4 shows Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The near infrared emission spectrum of the sample under the excitation of 1064nm laser is shown in the figure, and the near infrared emission spectrum has two different emission peaks of 1346nm and 1412nm respectively, and the full width at half maximum of the emission band is 265nm.
FIG. 5 shows Y obtained in example 2 2 Mg 0.99 Ni 0.01 TiO 6 The near infrared emission spectrum of the sample under the excitation of 1064nm laser can be seen from the figure, the two different emission peaks are respectively positioned at 1342nm and 1406nm, and the full width at half maximum of the emission band is 250nm.
FIG. 6 shows Y obtained in example 3 2 Mg 0.99 Ni 0.08 TiO 6 The near infrared emission spectrum of the sample under the excitation of 1064nm laser can be seen from the figure, the two different emission peaks are respectively positioned at 1346nm and 1425nm, and the full width at half maximum of the emission band is 255nm.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
Preparation of Y 2 Mg 0.96 Ni 0.04 TiO 6 Material
According to the chemical component general formula Y 2 Mg 0.96 Ni 0.04 TiO 6 Weighing raw materials of yttrium oxide 2.2581g, magnesium oxide 0.3868g, nickel oxide 0.0298g and titanium oxide 0.799g according to the corresponding stoichiometric ratio, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture for about 10 hours at 1400 ℃, naturally cooling, discharging and crushing to obtain the required fluorescent material.
Y prepared in this example 2 Mg 0.96 Ni 0.04 TiO 6 The absorption spectrum of the phosphor is shown in FIG. 1, the absorption peaks are 440nm,675nm and 1180nm, and are derived from octahedral hexa-coordinated Ni 2+ Electronic transitions of the ions. FIGS. 2, 3 and 4 show different embodimentsY under waveband excitation 2 Mg 0.96 Ni 0.04 TiO 6 The fluorescence spectrum of the fluorescent powder shows that the sample has broadband near-infrared luminescence at 1100-1700nm and is derived from eight-coordinate Ni 2+ Ion(s) 3 T 2 g(F)→ 3 A 2 g (F) electron transition.
FIG. 2 shows the fluorescence spectrum of the luminescent phosphor material prepared in this example under the excitation of 455nm semiconductor laser, which has two different emission peaks of 1348nm and 1420nm, respectively, and an emission band of 260nm at full width at half maximum.
FIG. 3 shows the fluorescence spectrum of the luminescent phosphor material prepared in this example under the excitation of 980nm semiconductor laser, which shows that it has two different emission peaks 1346nm and 1408nm, respectively, and the full width at half maximum of the emission band is 230nm.
FIG. 4 shows the fluorescence spectrum of the luminescent phosphor material prepared in this example under the excitation of 1064nm semiconductor laser, which shows that it has two different emission peaks of 1346nm and 1412nm, and the full width at half maximum of the emission band is 265nm.
Example 2
Preparation of Y 2 Mg 0.99 Ni 0.01 TiO 6 Material
According to the chemical component general formula Y 2 Mg 0.99 Ni 0.01 TiO 6 Weighing raw materials of yttrium oxide 2.2581g, magnesium oxide 0.3989g, nickel oxide 0.0074g and titanium oxide 0.799g according to the corresponding stoichiometric ratio, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture for about 10 hours at 1400 ℃, naturally cooling, discharging and crushing to obtain the required fluorescent material. The fluorescence spectrum of the fluorescent material under 1064nm excitation is shown in FIG. 5, two different emission peaks are respectively located at 1342nm and 1406nm, and the full width at half maximum of the emission band is 250nm.
Example 3
Preparation of Y 2 Mg 0.99 Ni 0.08 TiO 6 Material
According to the chemical component general formula Y 2 Mg 0.99 Ni 0.01 TiO 6 Weighing raw materials of yttrium oxide 2.2581g, magnesium oxide 0.3707g, nickel oxide 0.0597g and titanium oxide 0 according to the corresponding stoichiometric ratio799g, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture at 1400 ℃ for about 10 hours, naturally cooling, discharging and crushing to obtain the required fluorescent material. The fluorescence spectrum of the fluorescent material under 1064nm excitation is shown in FIG. 6, two different emission peaks are respectively located at 1346nm and 1425nm, and the full width at half maximum of the emission band is 255nm.
Example 4
Preparation of Gd 2 Mg 0.99 Ni 0.01 TiO 6 Material
According to the chemical component general formula Gd 2 Mg 0.99 Ni 0.01 TiO 6 Weighing raw materials of gadolinium oxide 3.6249g, magnesium oxide 0.3989g, nickel oxide 0.0074g and titanium oxide 0.799g according to the corresponding stoichiometric ratio, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture for about 10 hours at 1400 ℃, naturally cooling, discharging and crushing to obtain the required fluorescent material. Two different emission peaks are respectively positioned at 1346nm and 1418nm under the excitation of 455nm, and the full width at half maximum of an emission band is 250nm.
Example 5
Preparation of Gd 2 Mg 0.97 Ni 0.03 TiO 6 Material
According to the chemical composition general formula Gd 2 Mg 0.97 Ni 0.03 TiO 6 Weighing raw materials of gadolinium oxide 3.6249g, magnesium oxide 0.3909g, nickel oxide 0.0224g and titanium oxide 0.799g according to the corresponding stoichiometric ratio, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture for about 10 hours at 1450 ℃, naturally cooling, discharging and crushing to obtain the required fluorescent material. Two different emission peaks are respectively positioned at 1342nm and 1410nm under the excitation of 455nm, and the full width at half maximum of an emission band is 260nm.
Example 6
Preparation of Gd 2 Mg 0.92 Ni 0.08 TiO 6 Material
According to the chemical composition general formula Gd 2 Mg 0.99 Ni 0.01 TiO 6 Weighing raw materials of gadolinium oxide 3.6249g, magnesium oxide 0.3707g, nickel oxide 0.0597g and titanium oxide 0.799g according to the corresponding stoichiometric ratio, fully mixing and stirring, grinding for 1 hour, calcining the obtained mixture for about 10 hours at 1400 ℃, and naturally calcining for about 10 hoursCooling, discharging and crushing to obtain the required fluorescent material. Under the excitation of 455nm, two different emission peaks are respectively positioned at 1346nm and 1420nm, and the full width at half maximum of an emission band is 255nm.
Claims (9)
1. A broadband near-infrared luminescent material is characterized in that a double perovskite structure A is adopted 2 Mg 1-x TiO 6 Is matrix, wherein A is Y or Gd, and transition metal Ni is utilized 2+ The ions show broadband near-infrared luminescence in an octahedral hexa-coordinate environment, and the chemical composition general formula of the obtained material is A 2 Mg 1-x TiO 6 ：xNi 2+ Wherein x is more than or equal to 0.01 and less than or equal to 0.08.
2. The method for preparing the broadband near-infrared luminescent material of claim 1, comprising the steps of:
(1) Weighing: according to the chemical component general formula A 2 Mg 1-x TiO 6 ：xNi 2+ Wherein A is Y or Gd, x is more than or equal to 0.01 and less than or equal to 0.08, and raw materials of yttrium oxide, gadolinium oxide, magnesium oxide, titanium dioxide and nickel oxide are weighed according to the corresponding stoichiometric ratio in the formula;
(2) Mixing materials: uniformly mixing the weighed raw materials, and grinding to obtain a mixture;
(3) And (3) calcining: calcining the mixture obtained in the step (2);
(4) And naturally cooling, discharging and crushing to obtain the broadband near-infrared luminescent material.
3. The method for preparing a broadband near-infrared luminescent material according to claim 2, wherein in the step (2), the grinding time is 0.5 to 3 hours.
4. The method for preparing a broadband near-infrared luminescent material according to claim 2, wherein in the step (2), the grinding time is 1 to 2 hours.
5. The method for preparing a broadband near-infrared luminescent material according to claim 2, wherein in the step (3), the calcination temperature is 1200 to 1600 ℃.
6. The method for preparing a broadband near-infrared luminescent material according to claim 2, wherein in the step (3), the calcination temperature is 1300-1500 ℃.
7. The method for preparing a broadband near-infrared luminescent material according to claim 2, wherein in the step (3), the calcination temperature is 1400 to 1500 ℃.
8. Use of the broadband near-infrared luminescent material of claim 1 in a broadband near-infrared luminescent light source.
9. The application of the broadband near-infrared luminescent material obtained by the preparation method of any one of claims 2 to 7 in a broadband near-infrared luminescent light source.
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| Title |
|---|
| YUAN GAO ET AL.: "Near-infrared engineering for broad-band wavelength-tunable in biological window of NIR-II and -III: A solid solution phosphor of Sr1-xCaxTiO3:Ni2+", JOURNAL OF LUMINESCENCE, vol. 238, pages 118235 * |
| 高培鑫等: "新型植物补光用远红光(La, Gd, Y)2MgTiO6:Cr3+荧光粉的光谱调控", 发光学报, vol. 43, no. 1, pages 58 - 68 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116536043A (en) * | 2023-05-08 | 2023-08-04 | 昆明理工大学 | Near-infrared luminous perovskite fluorescent powder and preparation method and application thereof |
| CN116536043B (en) * | 2023-05-08 | 2024-03-12 | 昆明理工大学 | Near-infrared luminous perovskite fluorescent powder and preparation method and application thereof |
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| CN115717073B (en) | 2024-01-09 |
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