CN107118759B - Anti-hardening special-shaped composite luminescent powder and preparation method thereof - Google Patents
Anti-hardening special-shaped composite luminescent powder and preparation method thereof Download PDFInfo
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Abstract
The method co-assembles the precursor of the long-afterglow luminescent powder and the mesoporous silica precursor by a one-step method under the hydrothermal condition, takes the mesoporous silica material as a template, prepares the composite luminescent powder in a limited domain in a pore channel, regulates and controls the surface tension of the system by a composite solvent of palmitic acid and diacetone alcohol so as to control the morphology of the mesoporous silica, reduce the contact area between luminescent powder particles, relieve or even avoid the hardening phenomenon in the calcining process, and disperse the luminescent powder, thereby preparing the anti-hardening composite luminescent powder with excellent luminescent performance. The method has the advantages of simple preparation process, low cost and universality. The anti-hardening special-shaped composite luminescent powder can quickly absorb sunlight and slowly release under the irradiation of natural light, and can be used for illumination, emergency indication and the like in special environments.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to anti-hardening special-shaped composite luminescent powder and a preparation method thereof.
Background
The long afterglow luminescent material is a 'green' light source material, i.e. the light radiation energy is stored under the irradiation of natural light or artificial light source, and after the light source is cut off, the stored energy can be released in the form of visible light, so that it can present bright and distinguishable light, so that it is an ideal emergency indication light source. After hundreds of years of development, the long afterglow material has self-made a system, and shows wide application development prospects in various fields, especially in new fields such as biological imaging and the like, with unique 'charm' of the long afterglow material. At present, the method for preparing the rare earth long-afterglow luminescent material mainly comprises a combustion method, a sol-gel method, a chemical precipitation method, a hydrothermal method, a microemulsion method and the like.
However, the prior art is not enough to solve the serious agglomeration phenomenon of the luminescent nano-particles in the preparation process, and the luminescent and afterglow performances of the prepared luminescent nano-particles are not ideal. For example, in the preparation of rare earth long afterglow luminescent nano materials with high luminescent efficiency, the preparation of monodisperse nano particles is very difficult due to agglomeration and hardening of the materials in the sintering process. Therefore, how to prepare the monodisperse rare earth long afterglow luminescent nano particles with excellent luminescent property by a low-cost method has very important significance for further expanding the application range of the luminescent nano particles.
Disclosure of Invention
The invention aims to provide anti-hardening special-shaped composite luminescent powder with excellent luminescent property and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of anti-hardening special-shaped composite luminescent powder comprises the following steps:
s1, adding a nonionic surfactant P123 into the mixed solution of water and ethanol, adjusting the pH of the mixed solution to acidity by using hydrochloric acid, uniformly stirring, dropwise adding tetraethyl orthosilicate TEOS, and uniformly stirring to obtain a clear and transparent silicon dioxide precursor solution;
s2, dissolving strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate in a hydrochloric acid aqueous solution in proportion, dropwise adding the aqueous solution into the silicon dioxide precursor solution, adding a composite solvent of palmitic acid and diacetone alcohol to adjust the morphology of the product, uniformly stirring, transferring the product into a high-pressure reaction kettle of tetrafluoroethylene, and carrying out hydrothermal reaction at a proper temperature to obtain a precursor of the luminescent powder;
s3, washing the precursor of the reaction product, calcining in air atmosphere to remove organic species, and then using H2And (3) taking the/Ar mixed gas as a reducing atmosphere, controlling the heating speed in a tubular furnace, and calcining to obtain the anti-hardening special-shaped composite luminescent powder.
Further: in step S1, the ratio of the mixed solution of water and ethanol is within the range of 10:1 to 5: 1.
Further: in step S1, the content of the nonionic surfactant P123 is 0.5 wt% -8.0 wt%; the molar ratio of the hydrochloric acid to the TEOS is 1: 4-5: 1; the content of the TEOS is 0.5-1% of the volume of the solution.
Further: in step S1, the ratio of TEOS to strontium nitrate is 10: 1-20: 1.
Further: in the step S2, the molar ratio of the composite solvent of palmitic acid and diacetone alcohol to TEOS is 1: 5-1: 8; the nitrate ratio is 100:10:1: 2-80: 40:1: 2.
Further: in step S2, the hydrothermal reaction temperature is 140-160 ℃, and the reaction time is 12-24 hours.
Further: in step S3, the calcination temperature in the air atmosphere is controlled at 600 ℃, and the calcination time is 4 hours; the temperature rising speed in the tubular furnace is controlled to be 1-5 ℃/min, the calcining temperature in the tubular furnace is controlled to be 1300-1600 ℃, and the calcining time is 3-5 hours.
Further: the anti-hardening special-shaped composite luminescent powder is provided with dispersed luminescent nano-particles, the particle size of the luminescent nano-particles is 30-60 nm, and the monodispersion coefficient of the luminescent nano-particles is 0.05-0.1.
Further: the anti-hardening special-shaped composite luminescent powder is sea urchin-shaped, and the particle size of the anti-hardening special-shaped composite luminescent powder is 2-5 mu m.
Further: the anti-hardening special-shaped composite luminescent powder is prepared by the preparation method.
The invention has the beneficial effects that: the invention co-assembles the precursor of the long afterglow luminescent powder and the mesoporous silicon dioxide precursor by a one-step method under the hydrothermal condition, takes the mesoporous silicon dioxide material as a template, prepares the long afterglow material nano particles in the limited domain in the pore channel, and controls the mesoporous silicon dioxide to be sea urchin-shaped by regulating and controlling the surface tension of the system by the composite solvent of palmitic acid and diacetone alcohol. Therefore, the luminescent powder of the silicon-coated monodisperse rare earth long afterglow nano particles is prepared by one-step co-assembly, and the sea urchin-shaped luminescent powder obtained by shape regulation reduces the contact area among the luminescent powder particles, reduces the hardening phenomenon in the sintering process, is easier to disperse, so that the anti-hardening special-shaped composite luminescent powder with excellent luminescent performance is obtained.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
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FIG. 1 is an SEM photograph of sea urchin-shaped composite luminescent powder obtained by the preparation method shown in example 1 of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
(1) According to the molar ratio of TEOS: p123: HCl: h2O: preparing a mesoporous silica precursor solution from EtOH (1: 0.14:5.0:110: 11), adding a nonionic surfactant P123 into a mixed solution of 60ml of ethanol and water according to the proportion, adjusting the pH value by using hydrochloric acid, uniformly stirring, and then, dropwise adding tetraethoxysilane TEOS to obtain a clear and transparent silica precursor solution;
(2) and adding 10ml of a mixture aqueous solution of strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate into the silicon dioxide precursor solution, wherein the mass content of the strontium nitrate is 0.06, and the mass ratio of the strontium nitrate: magnesium nitrate: europium nitrate: dysprosium nitrate is mixed evenly in a mass ratio of 100:10:1:2, then 0.0125TEOS equivalent of composite solvent of palmitic acid and diacetone alcohol is added, the solution is transferred to a high-pressure reaction kettle of tetrafluoroethylene and reacts for 12 hours at a constant temperature of 140 ℃ to obtain a precursor of the rare earth long afterglow luminescent powder;
(3) washing the precursor with acetone, drying, heating to 600 deg.C at a temperature rise rate of 2 deg.C/min in air atmosphere, maintaining for 4 hr, and coolingPost-reuse H2The sea urchin-shaped composite luminescent powder which has excellent luminescence property and the grain diameter of 3 mu m and is wrapped by luminescent grains with the grain diameter of 30nm is prepared by taking mixed gas of Ar 1:9 as reducing atmosphere, slowly calcining in a tube furnace at the controlled heating rate of 1 ℃/min and keeping at 1300 ℃ for 3 h.
Referring to fig. 1, an SEM photograph of the sea urchin-shaped composite luminescent powder obtained by the preparation method shown in example 1 of the present invention. As can be seen from the figure, the composite luminescent powder prepared by the preparation method is in a sea urchin shape, is uniformly dispersed, and has the particle size of 2-5 microns.
Example 2
(1) According to the molar ratio of TEOS: p123: HCl: h2O: preparing a mesoporous silica precursor solution from EtOH 1:2.05:5.0:110:11, adding a nonionic surfactant P123 into a mixed solution of 60ml of ethanol and water according to the proportion, adjusting the pH value by using hydrochloric acid, uniformly stirring, and then, dropwise adding tetraethoxysilane TEOS to obtain a clear and transparent silica precursor solution;
(2) and adding 10ml of a mixture aqueous solution of strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate into the silicon dioxide precursor solution, wherein the mass content of the strontium nitrate is 0.06, and the mass ratio of the strontium nitrate: magnesium nitrate: europium nitrate: dysprosium nitrate is mixed evenly in a mass ratio of 80:40:1:2, then 0.2TEOS equivalent of composite solvent of palmitic acid and diacetone alcohol is added, the solution is transferred to a high-pressure reaction kettle of tetrafluoroethylene and reacts for 24 hours at a constant temperature of 160 ℃ to obtain a precursor of the rare earth long afterglow luminescent powder;
(3) washing the precursor with acetone, drying, heating to 600 deg.C at a temperature rising rate of 5 deg.C/min in air atmosphere, maintaining for 4 hr, cooling, and adding H2The sea urchin-shaped composite luminescent powder which has excellent luminescence property and the particle size of 5 mu m and is wrapped by luminescent particles with the particle size of 60nm is prepared by taking mixed gas of Ar 1:9 as a reducing atmosphere, slowly calcining in a tube furnace at the temperature rise speed of 1 ℃/min and keeping the temperature for 5 hours at 1600 ℃.
Example 3
(1) According to the molar ratio of TEOS: p123: HCl: h2O: preparing mesoporous silica precursor solution according to the proportion that EtOH is 1:0.44:0.25:110:22Adding a nonionic surfactant P123 into 60ml of mixed solution of ethanol and water, adjusting the pH value by hydrochloric acid, uniformly stirring, and then, dripping tetraethyl orthosilicate TEOS to obtain clear and transparent silicon dioxide precursor solution;
(2) adding 15ml of a mixture aqueous solution of strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate into the silicon dioxide precursor solution, wherein the mass content of the strontium nitrate is 0.09, and the mass ratio of the strontium nitrate: magnesium nitrate: europium nitrate: dysprosium nitrate is mixed evenly in a mass ratio of 100:20:1:2, then 0.1TEOS equivalent of composite solvent of palmitic acid and diacetone alcohol is added, the solution is transferred to a high-pressure reaction kettle of tetrafluoroethylene and reacts for 13 hours at a constant temperature of 150 ℃ to obtain a precursor of the rare earth long afterglow luminescent powder;
(3) washing the precursor with acetone, drying, heating to 600 deg.C at a temperature rising rate of 5 deg.C/min in air atmosphere, maintaining for 4 hr, cooling, and adding H2The sea urchin-shaped composite luminescent powder which has excellent luminescence property and the particle size of 4 mu m and is coated with luminescent particles of 40nm is prepared by taking mixed gas of Ar 1:9 as reducing atmosphere, slowly calcining in a tube furnace at the controlled heating rate of 3 ℃/min and keeping at 1300 ℃ for 4 h.
Example 4
(1) According to the molar ratio of TEOS: p123: HCl: h2O: preparing a mesoporous silica precursor solution from EtOH 1:0.18:0.5:100:12, adding a nonionic surfactant P123 into a mixed solution of 60ml of ethanol and water according to the proportion, adjusting the pH value by using hydrochloric acid, uniformly stirring, and then, dropwise adding tetraethoxysilane TEOS to obtain a clear and transparent silica precursor solution;
(2) and adding 12ml of a mixture aqueous solution of strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate into the silicon dioxide precursor solution, wherein the mass content of the strontium nitrate is 0.06, and the mass ratio of the strontium nitrate: magnesium nitrate: europium nitrate: dysprosium nitrate is mixed evenly in a mass ratio of 100:10:1:2, then 0.1TEOS equivalent of composite solvent of palmitic acid and diacetone alcohol is added, the solution is transferred to a high-pressure reaction kettle of tetrafluoroethylene and reacts for 18 hours at a constant temperature of 150 ℃ to obtain a precursor of the rare earth long afterglow luminescent powder;
(3) c for the above precursorWashing ketone, drying, heating to 600 deg.C at a temperature rising rate of 5 deg.C/min in air atmosphere, maintaining for 4 hr, cooling, and adding H2The sea urchin-shaped composite luminescent powder which has excellent luminescence property and the particle size of 2 mu m and is wrapped by luminescent particles with the particle size of 60nm is prepared by taking mixed gas of Ar 1:9 as a reducing atmosphere, slowly calcining in a tube furnace at the temperature rise speed of 2 ℃/min and keeping at 1300 ℃ for 2 h.
In summary, the following steps: the invention co-assembles the precursor of the long afterglow luminescent powder and the mesoporous silicon dioxide precursor by a one-step method under the hydrothermal condition, takes the mesoporous silicon dioxide material as a template, prepares the long afterglow material nano particles in the limited domain in the pore channel, and controls the mesoporous silicon dioxide to be sea urchin-shaped by regulating and controlling the surface tension of the system by the composite solvent of palmitic acid and diacetone alcohol. Therefore, the luminescent powder of the silicon-coated monodisperse rare earth long afterglow nano particles is prepared by one-step co-assembly, and the sea urchin-shaped luminescent powder obtained by shape regulation reduces the contact area among the luminescent powder particles, reduces the hardening phenomenon in the sintering process, is easier to disperse, so that the anti-hardening special-shaped composite luminescent powder with excellent luminescent performance is obtained.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. The preparation method of the anti-hardening special-shaped composite luminescent powder is characterized by comprising the following steps:
s1, adding a nonionic surfactant P123 into the mixed solution of water and ethanol, adjusting the pH of the mixed solution to acidity by using hydrochloric acid, uniformly stirring, dropwise adding tetraethyl orthosilicate TEOS, and uniformly stirring to obtain a clear and transparent silicon dioxide precursor solution;
s2, dissolving strontium nitrate, magnesium nitrate, europium nitrate and dysprosium nitrate in a hydrochloric acid aqueous solution in proportion, dropwise adding the aqueous solution into the silicon dioxide precursor solution, adding a composite solvent of palmitic acid and diacetone alcohol to adjust the morphology of the product, uniformly stirring, transferring the product into a polytetrafluoroethylene high-pressure reaction kettle, and carrying out hydrothermal reaction at a proper temperature to obtain a precursor of the luminescent powder; wherein the molar ratio of the composite solvent of palmitic acid and diacetone alcohol to TEOS is 1: 5-1: 8, the hydrothermal reaction temperature is 140-160 ℃, and the reaction time is 12-24 hours;
s3, washing the precursor of the reaction product, calcining in air atmosphere to remove organic matter, and then using H2And (3) taking the/Ar mixed gas as a reducing atmosphere, controlling the heating speed in a tubular furnace, and calcining to obtain the anti-hardening special-shaped composite luminescent powder.
2. The method for preparing the hardening-prevention special-shaped composite luminescent powder according to claim 1, wherein in step S1, the molar ratio of water to ethanol in the mixed solution of water and ethanol is within a range of 10:1 to 5: 1.
3. The method for preparing the anti-hardening special-shaped composite luminescent powder according to claim 1, wherein in step S1, the content of the nonionic surfactant P123 is 0.5 wt% to 8.0 wt%; the molar ratio of the hydrochloric acid to the TEOS is 1: 4-5: 1.
4. The method for preparing the anti-hardening special-shaped composite luminescent powder according to claim 1, wherein the molar ratio of TEOS to strontium nitrate is 10: 1-20: 1.
5. The method for preparing the anti-hardening special-shaped composite luminescent powder according to claim 1, wherein in step S3, the calcination temperature in the air atmosphere is controlled at 600 ℃ and the calcination time is 4 hours; the temperature rising speed in the tubular furnace is controlled to be 1-5 ℃/min, the calcining temperature in the tubular furnace is controlled to be 1300-1600 ℃, and the calcining time is 3-5 hours.
6. The method for preparing the hardening prevention special-shaped composite luminescent powder according to claim 1, wherein the hardening prevention special-shaped composite luminescent powder contains dispersed luminescent nanoparticles, the particle size of the dispersed luminescent nanoparticles is 30-60 nm, and the monodispersion coefficient of the dispersed luminescent nanoparticles is 0.05-0.1.
7. The method for preparing the hardening prevention special-shaped composite luminescent powder according to any one of claims 1 to 6, wherein the hardening prevention special-shaped composite luminescent powder is sea urchin-shaped, and the particle size of the hardening prevention special-shaped composite luminescent powder is 2-5 μm.
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