CN115717073B - 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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- 239000000126 substance Substances 0.000 claims abstract description 16
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 39
- 239000004408 titanium dioxide Substances 0.000 claims description 28
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 9
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 9
- 239000011159 matrix material Substances 0.000 claims description 7
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 6
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- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 6
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a near infrared broadband luminescent material, a preparation method and application thereof. The chemical component general formula of the fluorescent luminescent material is A 2 Mg 1‑x TiO 6 ：Ni 2+ Wherein A is Y or Gd, 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 chemical component general formula, mixed and stirred, and prepared by adopting a high-temperature solid phase method, 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 display 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 emission.
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 refers to a small portion of electromagnetic waves with wavelengths ranging from 780 to 2526nm, and due to its invisible nature and strong penetrating power, near infrared light sources are receiving more and more attention, and have very wide application from near infrared spectrum to fields of optical communication, night vision, photodynamic therapy, biomedical imaging, etc. 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 preferred over near infrared one-region (NIR-I, 700-1000 nm) light due to the lower optical scattering coefficient. Near infrared two-region fluorescence has the advantages of low scattering in organisms, deep tissue penetration and high imaging resolution compared with near infrared one-region (NIR-I, 700-1000 nm), making it a very promising technology. In this respect, a wider near infrared light is required as a support for quantitative analysis and diagnostic techniques of near infrared light sources to obtain comprehensive chemical and physical information. There are two types of near infrared light sources currently available on the market, one is a thermal light source comprising a tungsten/halogen lamp and a spherical lamp, and although the thermal light source has an ultra-wide bandwidth, the thermal light source inevitably has the defects of large volume, high power consumption, limited service life, serious heat dissipation and the like. Another is non-thermal light sources like lasers and light emitting diodes, which also affect their application due to extremely narrow bandwidths and spectral instability. Therefore, the exploration of novel near infrared luminescent materials covering the wave band of 1100-1700nm has important significance.
The rare earth ion luminescence is from 4f-4f electron layer transition, and because the rare earth ion luminescence is shielded by the outermost electron layer, the luminescence bandwidth is greatly limited, and the ultra-wideband luminescence requirement cannot be met. The transition metal ion luminescence is derived from 3d electron layer transition, is obviously influenced by surrounding coordination fields, and can realize broadband luminescence in a near infrared band. The transition metal element capable of emitting light in the broadband of 1000-1700nm in the optical communication band is mainly concentrated in Cr 4+ 、Ni 2+ 、Mn 6+ 、V 2+ However, cr 4+ 、Mn 6+ 、V 2+ Valence state instability in the material, the valence state must be controlled to obtain the desired infrared active center, greatly limiting its application in gain materials.
Due to transition metal ion Ni 2+ Such that Ni 2+ The luminescence of ions in an octahedral hexacoordinated environment is generally controllable and has broadband absorption and emission properties in the near infrared region. While Ni 2+ The valence state of (C) is stable, no special atmosphere control is needed, compared with other transition metal elements, ni 2+ Has obvious advantages as a near infrared luminescence center. With respect to Ni 2+ The research of near infrared broadband luminescence of ions can be traced to the 60 th century at the earliest, takenobu Suzuki et al observed MgGa at room temperature 2 O 4 ：Ni 2+ Spinel has a very broad emission band in the range 1100nm-1600nm (Journal of Luminescence (2005) 265-270). Matuszewska and L.Marciniak at (Sr, ca, ba, mg) TiO 3 ：Ni 2+ The wide-band luminescence of 1100nm-1600nm is realized, and Ni is changed according to the matrix 2+ The emission peak of the ion is shifted by about 500nm (Journal of Luminescence (2020) 117221). Guanliang Yu et al reported broadband NIR emission (Ceramics International (2021) 776-781) with a center wavelength of 1430nm and a Full Width Half Maximum (FWHM) of 230nm in a Ni2+ ion doped perovskite NaSbO3 lattice. Cuiping Wang et al in Nickel doped Zn 1+y Sn y Ga 2-2y O 4 Broadband luminescence of 1100nm-1600nm was achieved in solid solution (J.Mater.chem.C, 2021,9,4583-4590). Feng Liu et al in Zn 3 Ga 2 Ge 2 O 10 :Ni 2+ Ultra-wide luminescence at 1050-1600nm is realized (adv. Optical mate. 2016,4, 562-566). Lifang Yuan et al in garnet solid solution Y 3 Al 2 Ga 3 O 12 Broadband luminescence is realized, the emission center of the broadband luminescence is 1450nm, and the maximum half-width is 300nm (ACS appl. Mater. Interface 2022,14, 4265-4275). E.Martins a Et al in BaLiF 3 :Ni 2+ Ultra-wide luminescence (Journal of Luminescence 62 (1994) 281-289) of 1100nm-2000nm is realized.
According to the research situation of the nickel-doped near-infrared luminescent fluorescent powder, most of the nickel-doped near-infrared luminescent fluorescent powder uses germanate or gallate as a matrix material, but the cost of the germanate or gallate is relatively high, and the cost of the titanate is low and the material is easy to obtain. Secondly, the nickel-doped near infrared luminous fluorescent powder synthesized based on various fluorides has wider luminous bandwidth, but the product can pollute the environment in the production and use processes. The invention is based on (Y, gd) 2 MgTiO 6 The substrate nickel-doped near infrared luminescent material increases the variety of the broadband near infrared luminescent fluorescent powder. Based on (Y, gd) 2 MgTiO 6 Doped Ni 2+ The near infrared fluorescent powder of the ions can be effectively excited by light sources of various wave bands. Compared with the material, the material emits light to cover the broadband of 1100-1700nm in the near infrared band, and has the advantages of low cost, easily available raw materials, simple process, environment-friendly production process, no waste gas and waste liquid emission and the like.
Disclosure of Invention
Aiming at the problems of high price of the existing germanate or gallate, environmental pollution caused by fluoride and the like, the development of the fluorescent powder which is low in price, pollution-free to the environment and has good broadband near infrared light-emitting characteristics is important. The broadband near infrared luminescent fluorescent powder material provided by the invention has stable chemical performance, and the absorption band covers a plurality of wave bands, so that the broadband near infrared luminescent fluorescent powder material can be effectively excited by light sources of a plurality of wave bands. Meanwhile, broadband luminescence covering the near infrared band 1100-1700nm can be realized, and the maximum half-width of the emission band is 270nm. The method has the advantages of low cost, easily available raw materials, simple process, environment-friendly production process, no exhaust gas and waste liquid emission and the like. Another object of the present invention is to provide a method for preparing the above broadband near infrared emitting 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 matrix, reuse of transition metal Ni 2+ The ion presents broadband near infrared luminescence in the octahedral hexacoordination 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) Sample weighing: according to the chemical composition 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 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: uniformly mixing the weighed raw materials, and grinding to obtain a mixture;
(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 grinding time is 0.5 to 3 hours, preferably 1 to 2 hours.
Further, in step (3), the calcination temperature is 1200 to 1600 ℃, preferably 1300 to 1500 ℃, more preferably 1400 to 1500 ℃.
The broadband near infrared luminescent material obtained by the method has an absorption band covering a plurality of broadband, and can be effectively excited by various light sources in the ranges of 300-500nm, 600-800nm and 900-1500 nm. Obviously can meet the excitation requirement of various common light sources such as an LED blue light source, an LED near infrared light source and the like. The luminescent powder can realize broadband luminescence covering the near infrared band 1100-1700nm, and the maximum half-width of the emission band is 270nm, thus being particularly suitable for manufacturing broadband near infrared luminescent light sources.
Compared with the prior art, the invention has the following beneficial effects:
(1) The broadband near infrared luminous fluorescent powder material has ultra-wide emission of 1100nm-1700nm, and the maximum half-width 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 fluorescent powder material is prepared by adopting a high-temperature solid-phase reaction method, has low cost, easily available raw materials and simple process, is environment-friendly in production process, and has no waste gas and waste liquid emission.
Drawings
FIG. 1 shows Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 Absorption spectrum of the fluorescent powder at 400nm-1650 nm.
FIG. 2 is the Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The sample has near infrared emission spectrum under 455nm laser excitation, which has two different emission peaks of 1348nm and 1420nm, respectively, and an emission band half width of 260nm.
FIG. 3 is Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The sample has near infrared emission spectrum under 980nm laser excitation, which has two different emission peaks of 1346nm and 1408nm respectively, and the half-width of the emission band is 230nm.
FIG. 4 is the Y obtained in example 1 2 Mg 0.96 Ni 0.04 TiO 6 The near infrared emission spectrum of the sample under 1064nm laser excitation is shown to have two different emission peaks of 1346nm and 1412nm respectively, and the half-width of the emission band of 265nm.
FIG. 5 is Y obtained in example 2 2 Mg 0.99 Ni 0.01 TiO 6 The near infrared emission spectrum of the sample under 1064nm laser excitation is shown to have two different emission peaks at 1342nm and 1406nm respectively, with half-height of the emission bandThe width was 250nm.
FIG. 6 is Y obtained in example 3 2 Mg 0.99 Ni 0.08 TiO 6 The near infrared emission spectrum of the sample under 1064nm laser excitation is shown to have two different emission peaks at 1346nm and 1425nm respectively, and the half-width of the emission band is 255nm.
Detailed Description
The present invention will be described in further detail with reference to the following 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 composition general formula Y 2 Mg 0.96 Ni 0.04 TiO 6 According to the corresponding stoichiometric ratio, 2.2581g of yttrium oxide, 0.3868g of magnesium oxide, 0.0298g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, ground for 1 hour, the obtained mixture is calcined for about 10 hours at 1400 ℃, naturally cooled, discharged and crushed, and the required fluorescent material is obtained.
Y prepared in this example 2 Mg 0.96 Ni 0.04 TiO 6 The absorption spectrum of the fluorescent powder is shown in figure 1, the absorption peaks are 440nm,675nm and 1180nm respectively, and the absorption peaks are derived from octahedral hexacoordinated Ni 2+ Electron transitions of ions. FIGS. 2, 3 and 4 illustrate Y under excitation of different wavebands according to an embodiment 2 Mg 0.96 Ni 0.04 TiO 6 The fluorescence spectrum of the fluorescent powder can be seen that the sample has broadband near infrared luminescence at 1100-1700nm and is derived from eight-coordinated Ni 2+ Ion(s) 3 T 2 g(F)→ 3 A 2 g (F) electron transition.
FIG. 2 is a fluorescence spectrum of the luminescent phosphor material prepared in this example under 455nm semiconductor laser excitation, which shows that the luminescent phosphor material has two different emission peaks of 1348nm and 1420nm, respectively, and an emission band half width of 260nm.
Fig. 3 shows fluorescence spectra of the luminescent phosphor material prepared in this example under 980nm semiconductor laser excitation, and it can be seen that the luminescent phosphor material has two different emission peaks of 1346nm and 1408nm, respectively, and the half width of the emission band is 230nm.
Fig. 4 shows fluorescence spectra of the luminescent phosphor material prepared in this example under 1064nm semiconductor laser excitation, which has two different emission peaks of 1346nm and 1412nm, respectively, and an emission band half width of 265nm.
Example 2
Preparation of Y 2 Mg 0.99 Ni 0.01 TiO 6 Material
According to the chemical composition general formula Y 2 Mg 0.99 Ni 0.01 TiO 6 According to the corresponding stoichiometric ratio, 2.2581g of yttrium oxide, 0.3989g of magnesium oxide, 0.0074g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, ground for 1 hour, the obtained mixture is calcined for about 10 hours at 1400 ℃, naturally cooled, discharged and crushed, and the required fluorescent material is obtained. The fluorescence spectrum under 1064nm excitation is shown in FIG. 5, two different emission peaks are respectively positioned at 1342nm and 1406nm, and the half-width 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 composition general formula Y 2 Mg 0.99 Ni 0.01 TiO 6 According to the corresponding stoichiometric ratio, 2.2581g of yttrium oxide, 0.3707g of magnesium oxide, 0.0597g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, ground for 1 hour, the obtained mixture is calcined for about 10 hours at 1400 ℃, naturally cooled, discharged and crushed, and the required fluorescent material is obtained. The fluorescence spectrum under 1064nm excitation is shown in FIG. 6, two different emission peaks are respectively positioned at 1346nm and 1425nm, and the half-width of the emission band is 255nm.
Example 4
Preparation of Gd 2 Mg 0.99 Ni 0.01 TiO 6 Material
Gd according to the chemical composition formula 2 Mg 0.99 Ni 0.01 TiO 6 According to the corresponding stoichiometric ratio, 3.6249g of raw materials of gadolinium oxide, 0.3989g of magnesium oxide, 0.0074g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, and ground for 1 hour to obtain a mixtureCalcining at 1400 deg.c for 10 hr, cooling naturally, 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 half-width of an emission band is 250nm.
Example 5
Preparation of Gd 2 Mg 0.97 Ni 0.03 TiO 6 Material
Gd according to the chemical composition formula 2 Mg 0.97 Ni 0.03 TiO 6 According to the corresponding stoichiometric ratio, 3.6249g of gadolinium oxide, 0.3909g of magnesium oxide, 0.0224g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, ground for 1 hour, the obtained mixture is calcined for about 10 hours at 1450 ℃, naturally cooled, discharged and crushed, and the required fluorescent material is obtained. Two different emission peaks are respectively positioned at 1342nm and 1410nm under the excitation of 455nm, and the half-width of an emission band is 260nm.
Example 6
Preparation of Gd 2 Mg 0.92 Ni 0.08 TiO 6 Material
Gd according to the chemical composition formula 2 Mg 0.99 Ni 0.01 TiO 6 According to the corresponding stoichiometric ratio, 3.6249g of gadolinium oxide, 0.3707g of magnesium oxide, 0.0597g of nickel oxide and 0.799g of titanium oxide are weighed, fully mixed and stirred, ground for 1 hour, the obtained mixture is calcined for about 10 hours at 1400 ℃, naturally cooled, discharged and crushed, and the required fluorescent material is obtained. Two different emission peaks are respectively positioned at 1346nm and 1420nm under the excitation of 455nm, and the half-width of an emission band is 255nm.
Claims (9)
1. A broadband near infrared luminescent material is characterized by adopting a double perovskite structure A 2 Mg 1-x TiO 6 Is a matrix, wherein A is Y or Gd, and the transition metal Ni is recycled 2+ The ion presents broadband near infrared luminescence in an octahedral hexacoordinated 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;
the preparation method of the broadband near infrared luminescent material comprises the following steps:
(1) Sample weighing: according to the chemical composition 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: uniformly mixing the weighed raw materials, and grinding to obtain a mixture;
(3) Calcining: calcining the mixture obtained in the step (2);
(4) Naturally cooling, discharging and crushing to obtain the broadband near infrared luminescent material.
2. The method for preparing the broadband near infrared light emitting material according to claim 1, comprising the steps of:
(1) Sample weighing: according to the chemical composition 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: uniformly mixing the weighed raw materials, and grinding to obtain a mixture;
(3) Calcining: calcining the mixture obtained in the step (2);
(4) Naturally cooling, discharging and crushing to obtain the broadband near infrared luminescent material.
3. The method for preparing a broadband near infrared light emitting 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 light emitting 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 light emitting 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 light emitting material according to claim 2, wherein in the step (3), the calcination temperature is 1300 to 1500 ℃.
7. The method for preparing a broadband near infrared light emitting 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. Use 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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| Near-infrared engineering for broad-band wavelength-tunable in biological window of NIR-II and -III: A solid solution phosphor of Sr1-xCaxTiO3:Ni2+;Yuan Gao et al.;Journal of Luminescence;第238卷;第118235页 * |
| 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.2022,第43卷(第1期),第58-68页. * |
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