CN113481006B - Near infrared broad spectrum fluorescent material and preparation method and application thereof - Google Patents
Near infrared broad spectrum fluorescent material and preparation method and application thereof Download PDFInfo
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- CN113481006B CN113481006B CN202110797630.6A CN202110797630A CN113481006B CN 113481006 B CN113481006 B CN 113481006B CN 202110797630 A CN202110797630 A CN 202110797630A CN 113481006 B CN113481006 B CN 113481006B
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Abstract
The invention relates to the technical field of luminescent materials, in particular to a near infrared broad spectrum fluorescent material, a preparation method and application thereof. The invention is disclosed inA near infrared broad spectrum fluorescent material is provided, which has a chemical formula shown in a formula (I); (M) 1 1‑m Cr m )M 2 O 4 Formula (I); wherein M is 1 Selected from Al, ga, sc or In, and necessarily comprising Al and/or Ga; m is M 2 The element is selected from Ta or Nb; m is more than or equal to 0.0001 and less than or equal to 0.1. The fluorescent material selects M with rigid structure 1 M 2 O 4 Matrix material Cr 3+ Ion doping has developed the high efficiency excitation by 460nm blue light, the emission peak is located at 820-920nm and can be changed continuously, and the luminous efficiency is high.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a near infrared broad spectrum fluorescent material, a preparation method and application thereof.
Background
Compared with the traditional near infrared light source, the near infrared light emitting diode (pc-NIR-LED) based on fluorescence conversion has the advantages of low cost, good stability, easy regulation and control and the like, and is widely applied to the fields of biological imaging, food quality inspection, night vision monitoring and the like. The specific application thereof may be divided according to wavelength, for example: in the field of biological imaging, near infrared light of 650-950nm and 1000-1400nm can penetrate deep tissues and generate an autofluorescence background of zero phonons, so that near infrared biological imaging has low signal-to-noise ratio and high sensitivity. In the field of food detection, food is irradiated by near infrared light with the wavelength of 650-1050nm, and the components and the content of the food can be determined according to the absorption of compounds in the food to specific wavelengths, so that the non-contact nondestructive food detection is realized. Near infrared light of 830nm and 940nm can be applied to night vision function cameras. In addition, near infrared light at 850nm may be applied to iris, face recognition, and AR/VR (augmented/virtual reality) technology; the 940nm near infrared light can be applied to the detection of blood oxygen content. It can be seen that pc-NIR-LEDs play an increasingly important role in modern life and advanced technology, while near infrared fluorescent conversion materials become key materials determining their application range and efficiency.
Currently, cr 3+ Activated near infrared broad spectrum fluorescent powder is widely studied due to the advantages of high efficiency and the like, but the material still has some problems in performance. For example, materials have been developed with peak wavelengths mostly centered within 800nm, with less material greater than 800 nm; less material with internal quantum efficiency higher than 80% and emission peak wavelength smaller than 800nm, and external quantum efficiency generally lower than 35%; the material with the peak wavelength of more than 800nm has poor thermal stability and generally lower internal quantum efficiency<80％). These problems severely restrict the application of near infrared fluorescent conversion materials. Therefore, the search and development of high-efficiency near infrared broad spectrum materials with peak wavelength larger than 800nm is an urgent and inherent requirement for the development of near infrared fluorescence conversion LED devices, and has important significance.
Disclosure of Invention
In view of the above, the invention provides a near infrared broad spectrum fluorescent material, a preparation method and application thereof, wherein the excitation peak wavelength of the fluorescent material is located in the wave band of 450-480nm, the emission peak wavelength is located in the wave band of 820-900nm and can be continuously changed, the luminous efficiency is high, and the requirements of development of a broad spectrum near infrared LED device can be met.
The specific technical scheme is as follows:
the invention provides a near infrared broad spectrum fluorescent material, which has a chemical formula shown in a formula (I);
(M 1 1-m Cr m )M 2 O 4 formula (I);
in the middle, M 1 Selected from Al, ga, sc or In, and necessarily comprising Al and/or Ga; m is M 2 The element is selected from Ta or Nb; m is more than or equal to 0.0001 and less than or equal to 0.1.
In the invention, the M 1 Preferably Ga; the M is 2 Is Ta; m is preferably: m is more than or equal to 0.001 and less than or equal to 0.05.
The invention also provides a preparation method of the near infrared broad spectrum fluorescent material, which comprises the following steps:
will contain M 1 Compounds, containing M 2 Grinding the compound and the Cr-containing compound, mixing, and sintering to obtain the near infrared broad spectrum fluorescent material;
the near infrared broad spectrum fluorescent material has a chemical formula shown in a formula (I);
(M 1 1-m Cr m )M 2 O 4 formula (I);
in the middle, M 1 Selected from Al, ga, sc or In, and necessarily comprising Al and/or Ga; m is M 2 The element is selected from Ta or Nb; m is more than or equal to 0.0001 and less than or equal to 0.1.
In the present invention, the M-containing 1 The compound is selected from aluminum oxide, aluminum hydroxide, aluminum nitrate, gallium oxide,One or more of gallium nitrate, scandium oxide, scandium nitrate, indium oxide and indium hydroxide;
the M contains 2 The compound is tantalum oxide and/or niobium oxide;
the Cr compound is chromium oxide or chromium nitrate.
In the invention, the sintering is carried out in air, the sintering temperature is 1200-1500 ℃ and the sintering time is 4-12 h;
after sintering, the method further comprises: crushing and grinding the sintered product.
The invention also provides a near infrared broad spectrum fluorescent material or application of the near infrared broad spectrum fluorescent material in a broad spectrum near infrared LED device.
The invention uses the optical active element Cr 3+ Dissolved in M 1 M 2 O 4 (M 1 =al, ga, sc, or In, and must contain Al and/or Ga; m is M 2 Ta or Nb) crystalline phase, when the composition contains Al or Ga, a completely new material system with high luminous efficiency, in which the excitation peak wavelength is located in the 450-480nm band, and the emission peak wavelength is located in the 820-900nm, can be obtained. Belongs to a new structure and new component compound and has potential application value.
The invention relates to Cr 3+ Separately doping M 1 M 2 O 4 (M 1 =al, ga, sc, or In, and must contain Al and/or Ga; m is M 2 =ta or Nb), or on the basis of this, the new-component fluorescent material formed by Ta/Nb component change and Al/Ga/Sc/In ratio change, and a mixture containing the above components as main components, all belong to the category to which this patent relates. However, M is preferable in the fluorescent material of the present invention in view of luminous efficiency 1 For Ga, the object is to emphasize that the Ga-containing component has higher luminous efficiency than the Al, sc, or In-containing component alone and the component composed of Al, sc, or In combination; preferably M 2 For Ta, the purpose is to emphasize that Ta-containing components have higher luminous efficiency than Nb-containing components.
The near infrared broad spectrum fluorescent material provided by the invention can realize the regulation and control of the luminescence peak position and the luminescence efficiency through the change of Ta/Nb components and the adjustment of Al/Ga/Sc/In proportion. The optimized luminous efficiency can reach 90%, which is far superior to the existing material system, and has great application potential.
From the above technical scheme, the invention has the following advantages:
1. the excitation peak wavelength of the near infrared broad spectrum fluorescent material provided by the invention is 450-480nm, so that the near infrared broad spectrum fluorescent material can be suitable for excitation of a blue light LED chip and has strong practicability.
2. The near infrared broad spectrum fluorescent material provided by the invention can efficiently emit near infrared light with the peak wavelength of about 820-920nm under the excitation of 460nm blue light, and can be used as the broad spectrum fluorescent powder for the near infrared LED with fluorescence conversion.
3. The near infrared broad spectrum fluorescent material provided by the invention has the advantages of cheap and easily obtained raw materials, low synthesis temperature, simple preparation process, no need of special reaction equipment and convenient industrial production.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained from these drawings without inventive faculty for a person skilled in the art.
FIG. 1 shows Ga in example 1 of the present invention 0.998 Cr 0.002 TaO 4 Is an X-ray powder diffraction pattern of (2);
FIG. 2 shows Ga in example 1 of the present invention 0.998 Cr 0.002 TaO 4 Is a single crystal;
FIG. 3 shows Ga in example 1 of the present invention 0.998 Cr 0.002 TaO 4 Is a spectrum of the emission spectrum of (a);
FIG. 4 shows Al in example 2 of the present invention 0.99 Cr 0.01 TaO 4 Is a single crystal;
FIG. 5 shows Al in example 2 of the present invention 0.99 Cr 0.01 TaO 4 Is provided.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the embodiments described below are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
According to the chemical formula Ga of fluorescent powder 0.998 Cr 0.002 TaO 4 Weigh 0.0499mol Ga 2 O 3 、0.0001mol Cr 2 O 3 、0.05mol Ta 2 O 5 The raw materials are all analytically pure, and are weighed, matched, fully ground, uniformly mixed, put into an alumina crucible for roasting, and the roasting temperature is 1450 ℃ for 12 hours. After cooling to room temperature, crushing, grinding, washing and other post-treatments are carried out on the product, thus obtaining the Ga compound with the chemical composition 0.998 Cr 0.002 TaO 4 The X-powder diffraction pattern (Cu target, lambda= 0.15406 nm) and GaTaO of the fluorescent powder 4 A standard card pair such as that shown in fig. 1 has an excitation spectrum (under 840nm monitoring) as shown in fig. 2. As can be seen from FIG. 1, the present example successfully produced Ga 0.998 Cr 0.002 TaO 4 The method comprises the steps of carrying out a first treatment on the surface of the As can be seen from FIG. 2, the fluorescent powder can be effectively excited by blue light and red light in the range of 400-800 nm, and the main excitation peak is located at 470nm. FIG. 3 shows Ga in the present embodiment 0.998 Cr 0.002 TaO 4 As can be seen from fig. 3, the emission spectrum covers 700-1100nm, with the main emission peak at 840nm. Under excitation of 460nm blue light, the quantum yield reached 92% (see table 1).
Example 2
According to the chemical formula Al of the fluorescent powder 0.99 Cr 0.01 TaO 4 Weighing 0.0495mol of Al 2 O 3 、0.0005mol Cr 2 O 3 、0.05mol Ta 2 O 5 The raw materials are all analytically pure, the raw materials are weighed, matched and fully ground, after being uniformly mixed,placing the mixture into an alumina crucible for roasting, wherein the roasting temperature is 1300 ℃ and the temperature is kept for 8 hours. After cooling to room temperature, crushing, grinding, washing and other post-treatments are carried out on the product, and the chemical composition of Al is obtained 0.99 Cr 0.01 TaO 4 The excitation spectrum (under 900nm monitoring) of the fluorescent powder is shown in fig. 4, and as can be seen from fig. 4, the fluorescent powder can be effectively excited by blue light and red light in the range of 400-800 nm, and the main excitation peak is located at 645nm. FIG. 5 shows Al in the present embodiment 0.99 Cr 0.01 TaO 4 As can be seen from fig. 5, the emission spectrum covers 700-1300nm with a main emission peak at 900nm. Under excitation with 460nm blue light, the quantum yield was 80% (see table 1).
Example 3
According to the chemical formula Ga of fluorescent powder 0.9998 Cr 0.0001 NbO 4 Weigh 0.04999mol Ga 2 O 3 、0.000005mol Cr 2 O 3 、0.05mol Nb 2 O 5 The raw materials are all analytically pure, and are weighed, matched and fully ground, and are put into an alumina crucible for roasting after being uniformly mixed, and the roasting temperature is 1500 ℃ and the temperature is kept for 4 hours. After cooling to room temperature, crushing, grinding, washing and other post-treatments are carried out on the product, thus obtaining the Ga compound with the chemical composition 0.9998 Cr 0.0001 NbO 4 The fluorescent powder has excitation spectrum (under 838nm monitoring) covering 400-800 nm range, can be effectively excited by blue light and red light in 400-800 nm range, and has main excitation peak at 468nm. Ga under 460nm blue excitation 0.9998 Cr 0.0001 NbO 4 The emission spectrum of (a) covers 700-1100nm with a main emission peak at 838nm and a quantum yield of 75% (see Table 1).
Example 4
According to the chemical formula Al of the fluorescent powder 0.94 Cr 0.06 NbO 4 Weigh 0.094mol Al (OH) 3 、0.003mol Cr 2 O 3 、0.05mol Nb 2 O 5 The raw materials are all analytically pure, and are weighed, matched, fully ground, uniformly mixed, put into an alumina crucible for roasting, and the roasting temperature is 1200 ℃ for 8 hours. After cooling to room temperature, crushing, grinding, washing and other post-treatments are carried out on the product to obtain the chemical groupBecomes Al 0.94 Cr 0.06 NbO 4 The fluorescent powder has an excitation spectrum (under 895nm monitoring) covering 400-800 nm, can be effectively excited by blue light and red light, and has a main excitation peak at 670nm. Under the excitation of 460nm blue light, al 0.94 Cr 0.06 NbO 4 The emission spectrum of (2) covers 700-1300nm with a main emission peak at 895nm and a quantum yield of 60% (see Table 1).
Example 5
According to the chemical formula Al of the fluorescent powder 0.4 Ga 0.52 Cr 0.008 TaO 4 Weighing 0.02mol of Al 2 O 3 、0.026Ga 2 O 3 、0.0004mol Cr 2 O 3 、0.05mol Ta 2 O 5 The raw materials are all analytically pure, and are weighed, matched, fully ground, uniformly mixed, put into an alumina crucible for roasting, and the roasting temperature is 1400 ℃ for 10 hours. After cooling to room temperature, crushing, grinding, washing and other post-treatments are carried out on the product, and the chemical composition of Al is obtained 0.4 Ga 0.52 Cr 0.008 TaO 4 The fluorescent powder has an excitation spectrum (under 900nm monitoring) covering 400-800 nm, can be effectively excited by blue light and red light in 400-800 nm, and has a main excitation peak at 470nm. Under the excitation of 460nm blue light, al 0.4 Ga 0.52 Cr 0.008 TaO 4 The emission spectrum of (2) covers 700-1300nm with a main emission peak at 900nm and a quantum yield of 72% (see Table 1).
Example 6
The chemical formula of the phosphor prepared as in example 5 is shown as: ga 0.6 Sc 0.38 Cr 0.02 TaO 4 The emission peak wavelength and quantum yield of the obtained phosphor are shown in table 1.
Example 7
The chemical formula of the phosphor prepared as in example 5 is shown as: ga 0.7 In 0.25 Cr 0.05 TaO 4 The emission peak wavelength and quantum yield of the obtained phosphor are shown in table 1.
Example 8
The chemical formula of the phosphor prepared as in example 5 is shown as：Al 0.8 In 0.12 Cr 0.08 Ta 0.5 Nb 0.5 O 4 The emission peak wavelength and quantum yield of the obtained phosphor are shown in table 1.
Example 9
The chemical formula of the phosphor prepared as in example 5 is shown as: al (Al) 0.2 Ga 0.794 Cr 0.006 Ta 0.2 Nb 0.8 O 4 The emission peak wavelength and quantum yield of the obtained phosphor are shown in table 1.
Example 10
The chemical formula of the phosphor prepared as in example 5 is shown as: al (Al) 0.5 Sc 0.4 Cr 0.1 Ta 0.8 Nb 0.2 O 4 The emission peak wavelength and quantum yield of the obtained phosphor are shown in table 1.
TABLE 1 emission peak positions and quantum yields of the phosphors of examples 1 to 10 under 460nm excitation
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. A near infrared broad spectrum fluorescent material is characterized by having a chemical formula shown in a formula (I); (M) 1 1-m Cr m )M 2 O 4 Formula (I);
wherein M is 1 Selected from Ga, sc, and necessarily comprising Ga; m is M 2 The element is Ta; wherein when M 1 When selected from Ga, m=0.002, and has the chemical formula Ga 0.998 Cr 0.002 TaO 4 When M 1 When selected from the combination of Ga and Sc, m=0.02, the chemical formula is Ga 0.6 Sc 0.38 Cr 0.02 TaO 4 。
2. A method for preparing the near infrared broad spectrum fluorescent material of claim 1, comprising the steps of:
will contain M 1 Compounds, containing M 2 Grinding the compound and Cr-containing compound, mixing, and sintering at 1450 deg.C or 1400 deg.C in air to obtain near infrared broad spectrum fluorescent material with molecular formula (M) 1 1-m Cr m )M 2 O 4 。
3. The method according to claim 2, wherein the sintering is performed for a period of 10 to 12 hours.
4. The method of claim 2, wherein the M-containing component comprises 1 The compound is one or more than two of gallium oxide, gallium nitrate, scandium oxide and scandium nitrate; the M contains 2 The compound is tantalum oxide; the Cr compound is chromium oxide or chromium nitrate.
5. The method of manufacturing according to claim 2, wherein after sintering, further comprising: crushing and grinding the sintered product.
6. The use of the near infrared broad spectrum fluorescent material of claim 1 in broad spectrum near infrared LED devices.
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| CN114316974B (en) * | 2021-12-07 | 2023-03-31 | 广东工业大学 | Multi-lattice near-infrared broad spectrum fluorescent material and preparation method and application thereof |
| CN115772403B (en) * | 2022-12-06 | 2023-09-29 | 广州医科大学 | Chromium-thulium co-doped blue-violet light-to-narrow spectrum near infrared fluorescent material, and preparation and application thereof |
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