CN112195025B - Long-life room temperature phosphorescent material based on phosphorus-aluminum composite carbon dots and preparation method thereof - Google Patents
Long-life room temperature phosphorescent material based on phosphorus-aluminum composite carbon dots and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a long-life room temperature phosphorescent material based on a phosphorus-aluminum composite carbon dot and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing triethylene glycol, orthophosphoric acid and aluminum isopropoxide in proportion, adding a template agent organic alcohol amine compound and hydrofluoric acid, and stirring to form gel; and (3) carrying out hydrothermal reaction on the gel in a closed hydrothermal reaction kettle, and then carrying out post-treatment. The invention is prepared by a hydrothermal reaction method, has simple and convenient operation process, mild reaction conditions, high yield and low production cost, and is suitable for industrial production. The room temperature phosphorescent material prepared by the method takes the phosphorus-aluminum compound as a matrix and the carbon dots as a luminescence center, and the carbon dots are embedded into the matrix through hydrogen bonds, so that quenching of triplet excitons in oxygen can be effectively inhibited, the long decay life can be realized, green phosphorescence with the decay life as long as 754.91ms can be emitted after ultraviolet light excitation is finished, the room temperature phosphorescent material has the advantages of long decay life and easiness in industrial production, and has great application value in the fields of information safety, digital encryption and the like.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a long-life room temperature phosphorescent material based on carbon dots of a phosphorus-aluminum compound and a preparation method thereof.
Background
The long-life room temperature phosphorescent material is a special luminescent material, can slowly emit long-life phosphorescence visible to naked eyes after the irradiation of visible light, ultraviolet rays, X rays, gamma rays and the like is stopped, has low production cost, is safe and nontoxic, and is widely applied to the fields of information safety, digital encryption, life science, photoelectric devices and the like.
The long-life room temperature phosphorescent material comprises inorganic and organic long-life room temperature phosphorescent materials. The inorganic long-life room temperature phosphorescent material consists of sulfide-doped lanthanide ions or oxides with doped rare earth ions as luminescent centers. Because rare earth ions or transition metal ions need to be doped, the rare earth ions or transition metal ions are expensive and have certain biotoxicity, and the application of the rare earth ions or transition metal ions is limited to a certain extent. Compared with traditional inorganic long-life room temperature phosphorescent materials, the history of organic long-life room temperature phosphorescent materials is much shorter. Research in recent years has focused more on metal-doped organic materials, which generally require expensive heterocyclic conjugated systems containing heteroatoms as raw materials, require complicated synthesis and purification methods in order to obtain products, and are difficult to satisfy industrial production. Therefore, development of a long-life room temperature phosphorescent material which is easily industrially produced and has good light emitting properties is urgently required.
The carbon dots are novel luminescent materials developed in recent years, and have wide application in the fields of biological imaging, medical diagnosis, photoelectric devices and the like due to the advantages of simple preparation and purification processes, stable photophysical and chemical properties, adjustable emission characteristics, easy functional modification, good water solubility and the like. For example, the Chinese patent "a long-life organic room temperature phosphorescent material and a preparation method and application thereof" (application number 201610931156.0) takes carbon quantum dots and urea as materials, and the long-life organic room temperature phosphorescent material is prepared by mixing and stirring the materials with water, heating and cooling, and the raw materials are pure organic, nontoxic, cheap and easily obtained, the reaction conditions are mild, the operation is easy, and the method is suitable for mass production; however, the preparation process and the prepared product have the following disadvantages: (1) the process is complex: the carbon quantum dots are prepared firstly in the first step, and then are compounded with the matrix urea in the second step to obtain the carbon quantum dot composite material; (2) the process has high energy consumption: in the preparation process, not only hydrothermal heating in a hydrothermal reaction kettle is needed, but also a second stage of microwave heating is needed, so that the energy consumption is high, and especially the microwave heating is inconvenient for industrial large-scale production; (3) the organic urea is used as a matrix, so that the stability of the material is poor, and the phosphorescence life of the prepared material is short and can only reach 720ms at most.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a long-life room temperature phosphorescent material based on carbon dots of a phosphorus-aluminum composite and a preparation method thereof.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows: a preparation method of a long-life room temperature phosphorescent material based on a phosphorus-aluminum composite carbon dot comprises the following steps:
s1) mixing triethylene glycol, orthophosphoric acid and aluminum isopropoxide according to the weight ratio of 5-15: 0.3 to 0.9: uniformly mixing the components in a mass ratio of 0.2 to 0.8, adding a template agent, and mixing and stirring the mixture until gel is formed;
s2) transferring the gel obtained in the step S1) to a polytetrafluoroethylene high-pressure reaction kettle, then putting the kettle into an oven for hydrothermal reaction to prepare an initial solution of a carbon point, wherein the temperature of the hydrothermal reaction is 160-220 ℃, the reaction time is 48-72h, and then carrying out post-treatment on the initial solution of the carbon point, wherein the specific method comprises the following steps: and (3) carrying out suction filtration and washing on the initial solution of the carbon dots to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite.
Further, the template agent comprises an organic alcohol amine compound and hydrofluoric acid, and the mixing mass ratio of the organic alcohol amine compound to the hydrofluoric acid is (0.5) - (1.3): 0.05 to 0.2.
Further, the organic alcohol amine compound is monoethanolamine, diethanolamine or triethanolamine.
The invention also provides the long-life room temperature phosphorescent material based on the carbon point of the phosphorus-aluminum composite, which is prepared by the preparation method of the long-life room temperature phosphorescent material based on the carbon point of the phosphorus-aluminum composite.
The invention also provides application of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite, and the application fields comprise information security, digital encryption, life science and photoelectric devices.
The invention has the following beneficial effects:
1) The long-life room temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots has the advantages of simple synthetic route, mild reaction conditions, simple and convenient operation process, high yield, no need of expensive raw materials and complex equipment, low cost and suitability for industrial production;
2) The long-life room temperature phosphorescent material based on the carbon point of the phosphorus-aluminum composite provided by the invention takes the phosphorus-aluminum composite as a matrix and the carbon point as a luminescence center, and the surface of the carbon point is provided with a large number of groups such as C = O, C = N and the like, so that the conversion of singlet excitons into triplet excitons is facilitated. Meanwhile, carbon dots can be embedded into a phosphorus-aluminum compound matrix through hydrogen bonds, quenching of triplet excitons in oxygen can be effectively inhibited, and long decay life is facilitated to realize;
3) The matrix used in the invention is an inorganic phosphorus-aluminum compound, the stability of the material is better, the service life is longer, the generation of carbon points and the synthesis of the matrix phosphorus-aluminum compound are simultaneously completed in one step in a hydrothermal reaction kettle, the energy consumption is low, the steps are few, the process is simpler, and the industrial scale production is convenient;
4) The long-life room temperature phosphorescent material based on the carbon dots of the phosphor-aluminum composite can emit green phosphorescence with the decay life of 754.91ms after being excited and stopped by ultraviolet light, and has longer decay life, better application effect and wider application range compared with the average phosphorescence life of 0.72s of the long-life organic room temperature phosphorescent material prepared by the Chinese patent with the application number of 201610931156.0, the long-life organic room temperature phosphorescent material prepared by the preparation method and the application thereof.
Drawings
FIG. 1 is a transmission electron microscope representation result of a long-life room temperature phosphorescent material based on carbon dots of a phosphor-aluminum composite prepared in example 1 of the present invention, wherein A is a transmission electron microscope image, and B is a high resolution transmission electron microscope image;
FIG. 2 is a particle size distribution diagram of a long-life room temperature phosphorescent material based on carbon dots of a phosphor-aluminum composite prepared in example 1 of the present invention;
FIG. 3 is an X-ray diffraction pattern of a long-life room temperature phosphorescent material powder based on carbon dots of a phosphorus-aluminum composite prepared in example 1 of the present invention;
FIG. 4 is an IR spectrum of a long-life room temperature phosphor powder based on carbon dots of a P-Al composite prepared in example 1 of the present invention;
FIG. 5 is a graph of the morphology and energy spectrum analysis of a long-life room temperature phosphorescent material based on carbon dots of a phosphor-aluminum composite prepared in example 1, wherein a and c are scanning electron micrographs, and b and d are corresponding X-ray energy spectrum analysis graphs;
FIG. 6 is the result of X-ray photoelectron spectroscopy analysis of the long-life room temperature phosphorescent material based on the carbon dots of the phosphor-aluminum composite prepared in example 1, wherein a is the X-ray photoelectron spectroscopy spectrum, and b-d are high-resolution C1s, N1s and P2P spectra in sequence;
FIG. 7 is a graph of phosphorescence spectrum at room temperature of a long-life phosphorescence material at room temperature based on carbon dots of a phosphor-aluminum composite prepared in example 1 of the present invention;
FIG. 8 is a graph showing the decay of the phosphorescence lifetime at room temperature of the long-life phosphorescence materials based on the carbon dots of the phosphor-aluminum composite prepared in examples 1, 4 and 5 of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail in the following with the accompanying drawings of the specification.
The experimental procedures used in the following examples are, unless otherwise specified, all conventional procedures and the reagents, methods and equipment used, unless otherwise specified, are all conventional in the art.
The invention provides a preparation method of a long-life room temperature phosphorescent material based on a phosphorus-aluminum composite carbon dot, which comprises the following steps:
s1) mixing triethylene glycol, orthophosphoric acid and aluminum isopropoxide according to the weight ratio of 5 to 15:0.3 to 0.9: uniformly mixing the components in a mass ratio of 0.2 to 0.8, adding a template agent, and mixing and stirring the mixture until a gel is formed;
wherein the template agent comprises an organic alcohol amine compound and hydrofluoric acid, and the mixing mass ratio of the organic alcohol amine compound to the hydrofluoric acid is 0.5-1.3: 0.05 to 0.2.
Further, the organic alcohol amine compound is monoethanolamine, diethanolamine or triethanolamine.
S2) transferring the gel obtained in the step S1) to a polytetrafluoroethylene high-pressure reaction kettle, then putting the kettle into an oven for hydrothermal reaction to prepare an initial solution of a carbon point, wherein the temperature of the hydrothermal reaction is 160-220 ℃, the reaction time is 48-72h, and then carrying out post-treatment on the initial solution of the carbon point, wherein the specific method comprises the following steps: and (3) carrying out suction filtration and washing on the initial solution of the carbon dots to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite.
The following is a detailed description of specific embodiments.
Example 1
The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite comprises the following steps:
(1) Measuring 11.64g of triethylene glycol, adding the triethylene glycol into the open beaker, placing the beaker on a magnetic stirrer, and starting the magnetic stirrer;
(2) Slowly adding 0.6g of orthophosphoric acid into the beaker in the step (1), and fully stirring to uniformly disperse the orthophosphoric acid in the triethylene glycol;
(3) Adding 0.5g of aluminum isopropoxide powder into the beaker in the step (2), and continuously stirring for 2 to 3 hours to completely dissolve the aluminum isopropoxide powder;
(4) Respectively adding 0.85g of monoethanolamine and 0.13g of hydrofluoric acid into the beaker in the step (3), and continuously stirring for 3 hours to form uniform gel;
(5) Transferring the gel obtained in the step (4) into a 200mL polytetrafluoroethylene high-pressure reaction kettle, putting the kettle into an oven, and reacting for 3 days at 180 ℃ to obtain an initial solution of carbon dots;
(6) And (4) carrying out suction filtration and washing on the initial solution of the carbon dots obtained in the step (5) to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots.
Example 2
The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite comprises the following steps:
(1) Measuring 5g of triethylene glycol, adding the triethylene glycol into an open beaker, placing the beaker on a magnetic stirrer, and starting the magnetic stirrer;
(2) Slowly adding 0.3g of orthophosphoric acid into the beaker in the step (1), and fully stirring to uniformly disperse the orthophosphoric acid in the triethylene glycol;
(3) Adding 0.2g of aluminum isopropoxide powder into the beaker in the step (2), and continuously stirring for 2 to 3 hours to completely dissolve the aluminum isopropoxide powder;
(4) Respectively adding 0.5g of monoethanolamine and 0.05g of hydrofluoric acid into the beaker in the step (3), and continuously stirring for 3 hours to form uniform gel;
(5) Transferring the gel obtained in the step (4) into a 200mL polytetrafluoroethylene high-pressure reaction kettle, putting the kettle into an oven, and reacting for 3 days at 160 ℃ to obtain an initial solution of carbon dots;
(6) And (4) carrying out suction filtration and washing on the initial solution of the carbon dots obtained in the step (5) to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots.
Example 3
The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite comprises the following steps:
(1) Measuring 15g of triethylene glycol, adding the triethylene glycol into an open beaker, placing the beaker on a magnetic stirrer, and starting the magnetic stirrer;
(2) Slowly adding 0.9g of orthophosphoric acid into the beaker in the step (1), and fully stirring to uniformly disperse the orthophosphoric acid in the triethylene glycol;
(3) Adding 0.8g of aluminum isopropoxide powder into the beaker in the step (2), and continuously stirring for 2 to 3 hours to completely dissolve the aluminum isopropoxide powder;
(4) Respectively adding 1.3g of monoethanolamine and 0.2g of hydrofluoric acid into the beaker in the step (3), and continuously stirring for 3 hours to form uniform gel;
(5) Transferring the gel obtained in the step (4) into a 200mL polytetrafluoroethylene high-pressure reaction kettle, putting the kettle into an oven, and reacting for 2 days at 220 ℃ to obtain an initial solution of carbon dots;
(6) And (4) carrying out suction filtration and washing on the initial solution of the carbon dots obtained in the step (5) to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots.
Example 4
The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite comprises the following steps:
(1) Measuring 6.2g of triethylene glycol, adding the triethylene glycol into an open beaker, placing the beaker on a magnetic stirrer, and starting the magnetic stirrer;
(2) Slowly adding 0.4 g of orthophosphoric acid into the beaker in the step (1), and fully stirring to uniformly disperse the orthophosphoric acid in the triethylene glycol;
(3) Adding 0.3g of aluminum isopropoxide powder into the beaker in the step (2), and continuously stirring for 2 to 3 hours to completely dissolve the aluminum isopropoxide powder;
(4) Respectively adding 0.6g of diethanolamine and 0.06g of hydrofluoric acid into the beaker in the step (3), and continuously stirring for 3 hours to form uniform gel;
(5) Transferring the gel obtained in the step (4) into a 200mL polytetrafluoroethylene high-pressure reaction kettle, putting the kettle into an oven, and reacting for 2 days at 200 ℃ to obtain an initial solution of carbon dots;
(6) And (5) carrying out suction filtration and washing on the initial solution of the carbon dots obtained in the step (5) to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots.
Example 5
The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite comprises the following steps:
(1) Measuring 13g of triethylene glycol, adding the triethylene glycol into an open beaker, placing the beaker on a magnetic stirrer, and starting the magnetic stirrer;
(2) Slowly adding 0.8g of orthophosphoric acid into the beaker in the step (1), and fully stirring to uniformly disperse the orthophosphoric acid in the triethylene glycol;
(3) Adding 0.7g of aluminum isopropoxide powder into the beaker in the step (2), and continuously stirring for 2 to 3 hours to completely dissolve the aluminum isopropoxide powder;
(4) Respectively adding 0.85g of triethanolamine and 0.13g of hydrofluoric acid into the beaker in the step (3), and continuously stirring for 3 hours to form uniform gel;
(5) Transferring the gel obtained in the step (4) into a 200mL polytetrafluoroethylene high-pressure reaction kettle, putting the kettle into an oven, and reacting for 3 days at 190 ℃ to obtain an initial solution of carbon dots;
(6) And (4) carrying out suction filtration and washing on the initial solution of the carbon dots obtained in the step (5) to obtain a white solid, and drying the white solid at room temperature to obtain the long-life room-temperature phosphorescent material based on the phosphorus-aluminum composite carbon dots.
Example 6: long-life room temperature phosphorescent material correlation characteristic test based on phosphorus-aluminum composite carbon dots
1. The long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite prepared in the embodiment 1 of the invention is subjected to structural analysis:
transmission electron microscopy characterization is carried out on the long-life room temperature phosphorescent materials based on the carbon dots of the phosphorus-aluminum composite prepared in examples 1-5, wherein a transmission electron microscopy image and a high-resolution transmission electron microscopy image of the long-life room temperature phosphorescent materials based on the carbon dots of the phosphorus-aluminum composite prepared in example 1 are respectively shown in FIG. 1A and FIG. 1B. As can be seen from the transmission electron micrograph shown in the figure 1A, the carbon dots are embedded into the discontinuous spaces of the phosphorus-aluminum composite matrix; from the high-resolution transmission electron microscope shown in FIG. 1B, the regular hexagonal structure of the carbon dots and the good crystalline carbon region can be clearly seen, but the sharp dot profile is difficult to observe, and it can be presumed that the carbon dots are formed by Csp 2 And (4) forming.
The long-life room temperature phosphor material based on the carbon dots of the phosphor-aluminum composite prepared in example 1 is detected by a transmission electron microscope, and the particle size distribution range is mainly 2 to 6nm and the average particle size is 3.75nm by calculating the size of 100 carbon dots (see fig. 2).
The long-life room temperature phosphorescent materials based on the carbon dots of the phosphorus-aluminum composite prepared in examples 1 to 5 were subjected to X-ray diffraction analysis, wherein the X-ray diffraction pattern of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite prepared in example 1 is shown in fig. 3. From the X-ray diffraction pattern, it can be seen that the prepared long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum complex has low crystallinity, and the matrix does not have a complete zeolite structure, indicating that it does not completely form the aluminum phosphate zeolite, but is a phosphorus-aluminum complex.
The long-life room temperature phosphorescent materials based on the carbon dots of the phosphorus-aluminum composite prepared in examples 1 to 5 were subjected to infrared analysis, wherein an infrared spectrum of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite prepared in example 1 is shown in fig. 4. The infrared spectrum shows that the infrared spectrum is 3100cm -1 The characteristic peaks near are due to carboxylic acid groups at the carbon sites, at 3000cm -1 The nearby carbon point skeleton is in stretching vibration of 1650cm -1 Around C = O stretching vibration at carbon point, 1480cm -1 Around C = N,1050cm -1 The vicinity is C-O/C-N, indicating that the CDs generated contain abundant C = O/C = N.
The long-life room temperature phosphorescent materials based on the carbon dots of the phosphor-aluminum composite prepared in the above examples 1 to 5 were subjected to scanning electron microscope analysis and X-ray energy spectrum analysis, wherein the scanning electron microscope images of the long-life room temperature phosphorescent materials based on the carbon dots of the phosphor-aluminum composite prepared in example 1 are shown in fig. 5a and 5c, and the corresponding X-ray energy spectrum analysis images are shown in fig. 5b and 5 d. According to the scanning electron microscope image and the X-ray energy spectrum analysis image, the long-life room temperature phosphorescent material matrix based on the carbon dots of the phosphorus-aluminum composite has two structures, one is amorphous, the other is similar to a molecular sieve structure, and the result is consistent with the X-ray diffraction analysis.
The long-life room temperature phosphorescent materials based on carbon dots of the phosphor-aluminum composite prepared in the above examples 1 to 5 were subjected to X-ray photoelectron spectroscopy. The X-ray photoelectron spectrum and the high-resolution C1s, N1s and P2P spectra of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite prepared in example 1 are shown in fig. 6. According to the X-ray photoelectron spectrum and the high-resolution C1s, N1s and P2P energy spectrums, the long-life room-temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite contains C-O, C = C, C = O and P = O.
2. The long-life room-temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite is subjected to optical property analysis:
the long-life room temperature phosphorescent materials based on the carbon dots of the phosphor-aluminum composite prepared in the above examples 1 to 5 were subjected to room temperature phosphorescence spectrum analysis. The graph of the phosphorescence spectrum at room temperature (the inset is the image of the phosphorescence material at room temperature under white light, when the 365nm ultraviolet lamp is turned on and after being turned off) of the long-life room temperature phosphorescence material based on the carbon dots of the phosphor-aluminum composite prepared in example 1 is shown in fig. 7. As can be seen from the room temperature phosphorescence spectrogram, the phosphorescence emission wavelength of the long-life room temperature phosphorescence material based on the carbon dots of the phosphor-aluminum composite is 510nm.
The long-life room temperature phosphorescent materials based on the carbon dots of the phosphor-aluminum composite prepared in the above examples 1 to 5 were subjected to room temperature phosphorescence lifetime decay curve analysis to investigate the influence of the component ratio of the phosphor-aluminum composite and the template agent and the hydrothermal reaction conditions on the phosphorescence lifetime of the room temperature phosphorescent material in the preparation process. The decay curve of the phosphorescence lifetime at room temperature of the long-life room temperature phosphorescence materials based on the carbon dots of the phosphor-aluminum composites prepared in examples 1, 4 and 5 is shown in fig. 8. From the room temperature phosphorescence lifetime decay curve chart, the decay lifetime of the long-life room temperature phosphorescence material based on the phosphorus-aluminum composite carbon dot with the template agent of monoethanolamine is 754.91ms, which is the longest room temperature phosphorescence lifetime reported by the phosphorus-aluminum composite as the matrix and the carbon dot as the luminescence center, and the decay lifetimes of the long-life room temperature phosphorescence materials based on the phosphorus-aluminum composite carbon dot with the template agents of diethanolamine and triethanolamine are 730ms and 732.12ms, respectively.
According to the analysis results, the room-temperature phosphorescent material prepared by the hydrothermal method has good optical performance and long attenuation life by taking the phosphorus-aluminum compound as the matrix and taking the carbon dots as the luminescence center, can meet the requirements of people on the room-temperature phosphorescent material at present, and can be applied to the fields of information safety, digital encryption, life science, photoelectric devices and the like.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (5)
1. The preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite is characterized by comprising the following steps of:
s1) mixing triethylene glycol, orthophosphoric acid, aluminum isopropoxide and a template agent and stirring until gel is formed; the mixing mass ratio of the triethylene glycol to the orthophosphoric acid to the aluminum isopropoxide is 5-15: 0.3 to 0.9:0.2 to 0.8; the template agent comprises an organic alcohol amine compound and hydrofluoric acid, wherein the mixing mass ratio of the organic alcohol amine compound to the hydrofluoric acid is (0.5-1.3): 0.05 to 0.2; the organic alcohol amine compound is monoethanolamine, diethanolamine or triethanolamine;
and S2) placing the gel obtained in the step S1) in a closed environment for hydrothermal reaction, and then carrying out post-treatment to obtain the long-life room-temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite.
2. The method for preparing the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite as claimed in claim 1, wherein the method comprises the following steps: in the step S2), the reaction temperature of the hydrothermal reaction is 160-220 ℃, and the reaction time is 48-72 h.
3. The method for preparing the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite as claimed in claim 2, wherein the method comprises the following steps: in the step S2), the gel obtained in the step S1) is transferred to a polytetrafluoroethylene high-pressure reaction kettle, and then the gel is placed in an oven for hydrothermal reaction to prepare an initial solution of carbon dots.
4. The method for preparing the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite as claimed in claim 3, wherein the method comprises the following steps: in step S2), the post-processing method is: the initial solution of carbon dots was washed with suction to give a white solid, which was then dried at room temperature.
5. The long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite prepared by the preparation method of the long-life room temperature phosphorescent material based on the carbon dots of the phosphorus-aluminum composite as claimed in any one of claims 1 to 4.
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| 基于微孔晶体的长余辉材料的制备与发光性能研究;张洪月;《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》;20191115(第11期);B020-75 * |
| 新型碳点@无机微孔复合材料的合成及其发光性能研究;刘健聪;《中国优秀博硕士学位论文全文数据库(博士)工程科技Ⅰ辑》;20180315(第03期);B020-7 * |
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