CN112625682A - Cr3+Doped phosphate-based far-red light-near infrared luminescent material and preparation method thereof - Google Patents
Cr3+Doped phosphate-based far-red light-near infrared luminescent material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses Cr3+A doped phosphate-based far-red light-near infrared luminescent material and a preparation method thereof, the chemical composition formula is M9A1‑x(PO4)7:xCr3+Wherein M is at least one of Ca and Sr, A is at least one of Al, Ga, Sc, In, Lu and Y, and x is more than 0 and less than or equal to 1; belonging to beta-Ca3(PO4)2And (5) structure. The luminescent material is synthesized by a high-temperature solid phase method, the excitation wavelength range covers 250-800nm, 3 excitation peaks exist, the luminescent material can be simultaneously excited by blue light, green light and red light to realize far-red light-near infrared emission, and the emission wavelength range is 600-1100 nm. The luminescent material can be used for manufacturing far-red light-near infrared luminescent devices by matching with blue light, green light or red light LED chips, and can be used for plant growth, night vision imaging, agricultural product nondestructive quality analysis, human physiological state non-invasive detection, tracing marking and preventionThe fields of fake and the like have important application value. The preparation method has simple process and low raw material price, and is easy for large-scale technical popularization.
Description
Technical Field
The invention relates to the technical field of far-red light-near infrared luminescent materials, in particular to Cr3+A doped phosphate-based far-red light-near infrared luminescent material and a preparation method thereof.
Background
Far-red light (FR) refers to electromagnetic waves with a wavelength range of 650-780nm, and near-infrared light (NIR, 780-2526nm) is electromagnetic waves between visible light and mid-infrared light, and can be divided into two regions of near-infrared short wave (780-1100nm) and near-infrared long wave (1100-2526 nm). The near infrared spectrum belongs to the frequency doubling and dominant frequency absorption spectrum of molecular vibration spectrum, is generated when the molecular vibration transits from the ground state to the high energy level due to the non-resonance property of the molecular vibration, and has strong penetration capacity. Near-infrared light is mainly the frequency doubling and frequency combining absorption of the vibrations of hydrogen-containing groups X-H (X ═ C, N, O), and contains information on the composition and molecular structure of most organic compounds. Because different organic matters contain different groups, different groups have different energy levels, different groups and the same group have obvious difference on the absorption wavelength of near infrared light in different physical and chemical environments, and the near infrared spectrum can be used as an effective carrier for acquiring information, and has small absorption coefficient and less heat generation. When the organism is irradiated by near infrared light, light with the same frequency and radicals generate resonance phenomenon, and the energy of the light is transferred to molecules through the change of dipole moment of the molecules; when the frequency of the light is different from the vibration frequency of the organism, the light of the frequency is not absorbed. Therefore, when the organism is irradiated by near infrared light emitted by a wide spectrum, the near infrared light passing through the organism is weakened in certain wavelength ranges due to the selective absorption of different components to the near infrared light with different frequencies, and the transmitted near infrared light carries the component and the structural information of the organism.
The far-infrared light and the near-infrared light have important application values in the fields of plant growth, night vision imaging, agricultural product nondestructive quality analysis, human physiological state non-invasive detection, tracing marking, anti-counterfeiting and the like. The short wavelength near infrared light can penetrate food and is selectively absorbed by molecular vibration mode (C-H, N-H, O-H bond) in food, so that the food quality monitoring instrument can be used for monitoring the composition and quality information of vegetables and fruits in real time, and can be used for rapidly identifying the quality of food, distinguishing food and additives and the like. In addition, the biological optical window is provided with a first window (650-. In the aspect of plant growth, far-red light with the emission wavelength range of 700-740nm is used as a light source of a plant lamp, and the absorption of plant Pigments (PFR) can be promoted, so that the flowering period is shortened; meanwhile, the far-infrared light and the near-infrared light with the wavelength range of 715-1050nm can be absorbed by chlorophyll so as to promote the propagation of photosynthetic bacteria and further indirectly promote the growth of plants. It has been reported that infrared irradiation of rice hulls enhances the antioxidant activity of food and increases the nutritional value of food. Therefore, the far-infrared and near-infrared light sources with the wavelength range of 650-1100nm matched with the silicon detector have important application value. However, the conventional light sources such as incandescent lamps, halogen lamps and AlGaAs-based LEDs have the disadvantages of large size, short lifetime, low luminous efficiency, high operating temperature, narrow emission half-peak width (less than 50nm), and the like, which further limits the applications; therefore, the research and development of far-infrared and near-infrared luminescent materials capable of realizing efficient broadband emission are very important.
The luminescent material is composed of a matrix and an activator together. The trivalent chromium ion is the most ideal activator for realizing broadband far-red light-near infrared light luminescence, because of Cr3+The 3d orbit of the ion is greatly influenced by the external crystal field environment when Cr is3+When the ions are in a weak crystal field environment, to4T2→4A2Mainly broadband emission of; when Cr is present3+When the ions are in a strong crystal field environment, to2E→4A2Mainly narrow-band emission of. In addition, beta-Ca3(PO4)2The structural compound is a good matrix material, Ca has 5 different crystallographic lattice sites, and can form various types of compounds through cation substitution, and the structural compound has the advantages of stable chemical property, low raw material price, moderate synthesis temperature and the like. At present, the literature reports that a plurality of rare earth ions are doped with beta-Ca3(PO4)2Compounds of structure which can achieve visible light emission of different wavelengths, e.g. Sr8MgY(PO4)7:Eu2+(～610nm)，Sr8MgLu(PO4)7:Eu2+(～594nm)，Sr8ZnSc(PO4)7:Eu2+(～560nm)，Ca9Sc(PO4)7:Eu2+(～416nm)，Sr9Lu(PO4)7:Eu2+(～530nm)，Sr8ZnLu(PO4)7:Eu2+(～520nm)，Sr9Ga(PO4)7:Sm3+(～601nm)，Sr9Ga(PO4)7:Dy3+(～482nm)，Sr9Sc(PO4)7:Eu2+(～510nm)，Ca9Ga(PO4)7:Ce3+(～380nm)，Ca9In(PO4)7:Ce3+(～380nm)，Ca9Lu(PO4)7:Eu2+(～480nm)，Ca9Al(PO4)7:Ce3+(-365 nm), and the like. However, there is no report in the literature on β -Ca3(PO4)2The structural compound is doped with transition metal Cr3+Ions are used for realizing far-red light-near infrared light emission and manufacturing a novel light-emitting device, so that the research has important scientific significance and application value.
Disclosure of Invention
The invention aims to provide novel Cr3+The doped phosphate-based far-red light-near infrared luminescent material has an excitation wavelength range covering 250-800nm, has 3 excitation peaks, can be simultaneously excited by blue light, green light and red light to realize far-red light-near infrared emission, has an emission wavelength range of 600-1100nm, and can cover a bio-optical first window (650-950nm) and a second window (1000-1350 nm).
Another object of the present invention is to provide the above Cr3+The preparation method of the doped phosphate-based far-red light-near infrared luminescent material has simple preparation process and is easy for large-scale technical popularization.
The purpose of the invention is realized by the following technical scheme:
cr (chromium)3+Doped phosphate-based far-red light-a near-infrared luminescent material, characterized in that the luminescent material has a chemical composition formula of M9A1-x(PO4)7:xCr3+Wherein M is at least one of Ca and Sr, A is at least one of Al, Ga, Sc, In, Lu and Y, and x is more than 0 and less than or equal to 1; belonging to beta-Ca3(PO4)2And (5) structure.
Cr as described above3+The doped phosphate-based far-red-near-infrared luminescent material is characterized in that M element can be partially replaced by D element, and the chemical composition formula is M9-yDyA1-x(PO4)7:xCr3+D is at least one of Mg and Zn, and y is more than or equal to 0 and less than or equal to 1.
Cr as described above3+The preparation method of the doped phosphate-based far-red light-near infrared luminescent material is characterized by comprising the following steps:
(1) weighing materials: according to the chemical composition formula M9A1-x(PO4)7:xCr3+Proportioning according to stoichiometric ratio, and respectively weighing M-containing carbonate or oxide, A-containing oxide and NH4H2PO4And oxides containing Cr, fully grinding and uniformly mixing; or according to the chemical composition formula M9-yDyA1-x(PO4)7:xCr3+Proportioning according to stoichiometric ratio, and weighing M-containing carbonate or oxide, D-containing oxide, A-containing oxide and NH respectively4H2PO4And oxides containing Cr, fully grinding and uniformly mixing;
(2) placing the mixture obtained in the step (1) in an alumina crucible, calcining the mixture in a high-temperature furnace at the temperature of 500-900 ℃ for 2-6 hours at the heating rate of 2-10 ℃/min, cooling the mixture to room temperature along with the furnace, and grinding the sintered body into powder;
(3) and (3) placing the mixture obtained in the step (2) into an alumina crucible again, calcining the mixture in a high-temperature furnace at the temperature of 1000-1400 ℃ for 3-10 hours at the heating rate of 5-10 ℃/min, cooling the mixture to 800 ℃ at the cooling rate of 5-10 ℃/min, cooling the cooled mixture to room temperature along with the furnace, and grinding the sintered body into powder.
(4) And (4) carrying out a post-treatment process on the mixture obtained in the step (3) to remove impurities in a grading manner.
Cr as described above3+The preparation method of the doped phosphate-based far-red light-near infrared luminescent material is characterized in that in the step (4), the post-treatment process comprises crushing, airflow crushing, impurity removal, drying and grading; the grading process adopts at least one of a sedimentation method, a screening method, hydraulic grading and airflow grading; the impurity removal process comprises acid washing, alkali washing or water washing.
The Cr of the invention3+The doped phosphate-based far-red light-near infrared luminescent material can be prepared into a novel far-red light-near infrared luminescent material with the emission wavelength range of 600-1100nm by matching with organic materials, ceramics or glass; the luminescent material can be prepared into a novel luminescent device by matching with blue light, green light or red light LED chips, and can be used in the fields of plant growth, night vision imaging, nondestructive quality analysis of agricultural products, non-invasive detection of human physiological states, tracing marks, anti-counterfeiting and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the excitation wavelength coverage range is wide, 3 excitation peaks exist, and the excitation wavelength coverage range is matched with the emission wavelengths of the blue light LED chip, the green light LED chip and the red light LED chip;
(2) the emission spectrum is wide in coverage, can cover a biological optical first window and a biological optical second window, and has application value in multiple fields;
(3) the fluorescent material has high luminous efficiency and excellent thermal quenching characteristic;
(4) the physical and chemical properties are stable;
(5) the preparation method is simple, the raw materials are low in price, and the large-scale popularization is easy.
Drawings
Fig. 1 is a powder X-ray diffraction (XRD) pattern of a sample prepared in example 1 of the present invention.
FIG. 2 is a graph of the excitation spectrum of a sample prepared in example 1 of the present invention.
FIG. 3 is a graph of the emission spectrum of a sample prepared in example 1 of the present invention.
Fig. 4 is a powder X-ray diffraction (XRD) pattern of a sample prepared in example 2 of the present invention.
FIG. 5 is a graph of the excitation spectrum of a sample prepared in example 2 of the present invention.
Fig. 6 is an emission spectrum of a sample prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
This example has a chemical composition formula of Ca9Ga0.95(PO4)7:0.05Cr3+The preparation method of the far-red light-near infrared luminescent material comprises the following steps:
according to the chemical composition formula Ca9Ga0.95(PO4)7:0.05Cr3+Stoichiometric ratio, separately weighing CaCO3、Ga2O3、NH4H2PO4、Cr2O3Putting the high-purity powder raw material into an agate mortar, adding a proper amount of absolute ethyl alcohol, and grinding for 30 minutes to fully and uniformly mix the raw material. Then transferring the mixed raw materials into an alumina crucible, placing the alumina crucible into a high-temperature box type furnace, heating the alumina crucible to 800 ℃ at the heating rate of 3 ℃/min, calcining the alumina crucible for 4 hours, naturally cooling the alumina crucible, taking out the alumina crucible and grinding the alumina crucible into powder. Then transferring the ground mixture into an alumina crucible again, placing the alumina crucible into a high-temperature box type furnace, heating the alumina crucible to 1200 ℃ at the heating rate of 5 ℃/min, calcining the alumina crucible for 5 hours, cooling the alumina crucible to 800 ℃ at the cooling rate of 10 ℃/min, cooling the alumina crucible to room temperature along with the furnace, taking out the alumina crucible and grinding the alumina crucible to obtain the single-phase Ca9Ga0.95(PO4)7:0.05Cr3+Far-red light-near infrared luminescent material.
The far-red light-near infrared luminescent material prepared in this example has a powder X-ray diffraction (XRD) pattern as shown in fig. 1, an excitation spectrum as shown in fig. 2, and an emission spectrum as shown in fig. 3. The excitation wavelength range is 250-700nm, 3 excitation peaks are respectively located at 250-360nm, 360-530nm and 530-700nm, and the emission band is located at 600-850nm, so that the phosphate-based luminescent material can realize far-red light-near infrared emission.
Example 2
This example has a chemical composition formula of Sr9In0.9(PO4)7:0.1Cr3+The preparation method of the far-red light-near infrared luminescent material comprises the following steps:
according to the chemical composition formula Sr9In0.9(PO4)7:0.1Cr3+Stoichiometric ratio, respectively weighing SrCO3、In2O3、NH4H2PO4、Cr2O3Putting the high-purity powder raw material into an agate mortar, adding a proper amount of absolute ethyl alcohol, and grinding for 30 minutes to fully and uniformly mix the raw material. Then transferring the mixed raw materials into an alumina crucible, placing the alumina crucible into a high-temperature box type furnace, heating the alumina crucible to 750 ℃ at the heating rate of 4 ℃/min, calcining the alumina crucible for 3 hours, naturally cooling the alumina crucible, taking out the alumina crucible and grinding the alumina crucible into powder. Then transferring the ground mixture into an alumina crucible again, placing the alumina crucible into a high-temperature box type furnace, heating the alumina crucible to 1250 ℃ at the heating rate of 8 ℃/min, calcining the alumina crucible for 4 hours, cooling the alumina crucible to 800 ℃ at the cooling rate of 10 ℃/min, cooling the alumina crucible to room temperature along with the furnace, taking out the alumina crucible and grinding the alumina crucible to obtain single-phase Sr9In0.9(PO4)7:0.1Cr3+Far-red light-near infrared luminescent material.
The powder X-ray diffraction (XRD) pattern of the far-red-near-infrared luminescent material prepared in this example is shown in fig. 4, the excitation spectrum is shown in fig. 5, and the emission spectrum is shown in fig. 6. The excitation wavelength range is 250-800nm, 3 excitation peaks are respectively located at 250-360nm, 390-570nm and 570-800nm, and the emission band is located at 700-1100nm, so that the phosphate-based luminescent material can realize far-red light-near infrared emission.
Examples 3 to 22 desired raw materials were weighed according to the chemical composition formulas and stoichiometric ratios in table 1, the preparation method thereof was the same as in example 1, and the excitation peak wavelength ranges and emission wavelength ranges of the synthesized samples are listed in table 1.
TABLE 1
| Practice ofExample (b) | TransformingChemical compositionFormula (II) | LaserPeak generationWave (wave)Long range (nm) | LaunchingWave (wave)Long range (nm) |
| Ratio ofComparative example 1 | Ca9Ga0.95(PO4)7:0.05Cr3+ | 250-360,360-530,530-700 | 600-850 |
| 3 | Ca9Al0.8(PO4)7:0.2Cr3+ | 250-340,365-535,535-700 | 600-950 |
| 4 | Ca9Ga0.99(PO4)7:0.01Cr3+ | 250-360,360-530,530-700 | 600-870 |
| 5 | Ca9In0.9(PO4)7:0.1Cr3+ | 250-335,360-550,550-700 | 600-1000 |
| 6 | Ca9Sc0.7(PO4)7:0.3Cr3+ | 250-340,385-510,510-700 | 600-980 |
| 7 | Ca9Lu0.6(PO4)7:0.4Cr3+ | 250-345,380-540,540-700 | 600-1050 |
| 8 | Ca9Cr(PO4)7 | 250-330,360-530,530-700 | 650-1100 |
| 9 | Sr9In0.99(PO4)7:0.01Cr3+ | 250-360,390-570,570-800 | 700-1100 |
| 10 | Sr9Sc0.87(PO4)7:0.13Cr3+ | 250-365,385-570,570-800 | 670-1100 |
| 11 | Sr9Lu0.1(PO4)7:0.9Cr3+ | 250-370,400-575,575-800 | 690-1100 |
| 12 | Sr9Ga0.3(PO4)7:0.7Cr3+ | 250-375,385-570,570-800 | 630-1100 |
| 13 | Sr9Cr(PO4)7 | 250-370,390-565,565-800 | 650-1100 |
| 14 | Ca8MgSc0.5(PO4)7:0.5Cr3+ | 250-365,365-525,525-700 | 650-1100 |
| 15 | Ca8MgLu0.81(PO4)7:0.19Cr3+ | 250-340,370-530,530-700 | 650-1100 |
| 16 | Ca8MgY0.93(PO4)7:0.07Cr3+ | 250-330,380-545,545-700 | 650-1100 |
| 17 | Sr8MgSc0.7(PO4)7:0.3Cr3+ | 250-350,385-580,580-800 | 700-1100 |
| 18 | Sr8MgLu0.84(PO4)7:0.16Cr3+ | 250-355,375-575,575-800 | 700-1100 |
| 19 | Sr8MgY0.6(PO4)7:0.4Cr3+ | 250-360,385-570,570-800 | 700-1100 |
| 20 | Ca8ZnLu0.8(PO4)7:0.2Cr3+ | 250-400,400-550,550-800 | 650-1100 |
| 21 | Sr8ZnLu0.95(PO4)7:0.05Cr3+ | 250-365,395-580,580-800 | 720-1100 |
| 22 | Sr8ZnSc0.3(PO4)7:0.7Cr3+ | 250-360,390-590,590-800 | 700-1100 |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which are made without departing from the spirit and principle of the present invention should be regarded as equivalent replacements within the protection scope of the present invention.
Claims (8)
1. Cr (chromium)3+The doped phosphate-based far-red light-near infrared luminescent material is characterized in that the chemical composition formula of the luminescent material is M9A1-x(PO4)7:xCr3+Wherein M is at least one of Ca and Sr, A is at least one of Al, Ga, Sc, In, Lu and Y, and x is more than 0 and less than or equal to 1.
2. The Cr of claim 13+Doped phosphate-based far-red-near-infrared luminescent material, characterized in that the crystal structure type belongs to beta-Ca3(PO4)2And (5) structure.
3. The Cr of claim 13+The doped phosphate-based far-red-near infrared luminescent material is characterized in that the excitation wavelength range covers 250-800nm, 3 excitation peaks are provided, the far-red-near infrared luminescent material can be excited by blue light, green light and red light simultaneously to realize far-red-near infrared emission, and the emission wavelength range is 600-1100 nm.
4. The Cr of claim 13+The doped phosphate-based far-red-near-infrared luminescent material is characterized in that the emission wavelength covers a bio-optical first window (650-.
5. The Cr of claim 13+The doped phosphate-based far-red-near-infrared luminescent material is characterized in that M element can be partially replaced by D element, and the chemical composition formula is M9-yDyA1-x(PO4)7:xCr3+D is at least one of Mg and Zn, and y is more than or equal to 0 and less than or equal to 1.
6. The Cr of claim 13+The preparation method of the doped phosphate-based far-red light-near infrared luminescent material is characterized by comprising the following steps:
(1) weighing materials: according to the chemical composition formula M9A1-x(PO4)7:xCr3+Proportioning according to stoichiometric ratio, and respectively weighing M-containing carbonate or oxide, A-containing oxide and NH4H2PO4And oxides containing Cr, fully grinding and uniformly mixing; or according to the chemical composition formula M9-yDyA1-x(PO4)7:xCr3+Proportioning according to stoichiometric ratio, and weighing M-containing carbonate or oxide, D-containing oxide, A-containing oxide and NH respectively4H2PO4And oxides containing Cr, fully grinding and uniformly mixing;
(2) placing the mixture obtained in the step (1) in an alumina crucible, calcining the mixture in a high-temperature furnace at the temperature of 500-900 ℃ for 2-6 hours at the heating rate of 2-10 ℃/min, cooling the mixture to room temperature along with the furnace, and grinding the sintered body into powder;
(3) placing the mixture obtained in the step (2) in an alumina crucible again, calcining the mixture in a high-temperature furnace at the temperature of 1000-1400 ℃ for 3-10 hours at the heating rate of 5-10 ℃/min, cooling the mixture to 800 ℃ at the cooling rate of 5-10 ℃/min, cooling the mixture to room temperature along with the furnace, and grinding the sintered body into powder;
(4) and (4) carrying out a post-treatment process on the mixture obtained in the step (3) to remove impurities in a grading manner.
7. The Cr of claim 53+Doped phosphate-based far-red-near-infrared luminescent materialThe preparation method of the material is characterized in that in the step (4), the post-treatment process comprises crushing, airflow crushing, impurity removal, drying and classification; the grading process adopts at least one of a sedimentation method, a screening method, hydraulic grading and airflow grading; the impurity removal process comprises acid washing, alkali washing or water washing.
8. The Cr of claim 13+The doped phosphate-based far-red light-near infrared luminescent material is characterized in that the luminescent material can be prepared into a novel far-red light-near infrared luminescent material with the emission wavelength range of 600-1100nm by matching with organic materials, ceramics or glass; the luminescent material is matched with a blue light, green light or red light LED chip to prepare a novel luminescent device, and is used for the fields of plant growth, night vision imaging, nondestructive quality analysis of agricultural products, non-invasive detection of human physiological states, tracing marking and anti-counterfeiting.
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