CN1563271A - Long persistence phosphorescence material of nano aluminate and preparation method - Google Patents
Long persistence phosphorescence material of nano aluminate and preparation method Download PDFInfo
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Abstract
The chemical formula for long persistence lightening material of nanoaluminate is xMo.yAl2O3:Eu0.01x, Dy0.01x as M is Sr or Ca, x=1 y=1 or x=4 and y=7. The preparing method includes using Sr (NO3)2, Ca (NO3)2, 6H2O, Al(NO3)3.9H2O, (NH4)2CO3, Eu2O3, Dy2O3 H2BO3 and HNO3 as raw materials; dissolving Eu2O3 and Dy2O3 in HNO3 to form trivalent nitrate; dissolving Sr(NO3)2, Ca(NO3)2.6H2O and Al(NH3)3.9H2O in deionized water to form nitrate solution; precipitating with (NH4)2CO3 solution; ball-grinding precipited material and obtaining product through drying and calcining.
Description
Technical Field
The invention relates to a long afterglow luminescent material and a preparation method thereof, in particular to a nano aluminate long afterglow luminescent material and a preparation method thereof, which are used in the field of luminescent materials.
Background
The conventional sulfide series long afterglow luminescent materials are continuously improved to form several typical products, such as: ZnS: Cu (green luminescence), (CaSr) S: Bi (blue luminescence), (ZnCd) S: Cu (yellow orange luminescence). However, these materials have poor stability, are easily decomposed in air, are easily grayed to black under the irradiation of sunlight, have short luminescence afterglow time and have low luminescence brightness. To solve these problems, Co, Ra, and Ti were added to these materials,3Radioactive elements such as H, etc. are used to make long-afterglow radioactive material, but its application range is greatly limited because of radioactive pollution and high cost. Compared with sulfide, the aluminate long afterglow luminescent material is used as an energy-saving energy storage material, and is applied to the aspects of articles for daily use, low-degree illumination indication signs, clocks and watches and the like because of high luminous brightness, excellent long afterglow performance and better stability. The present aluminate luminescent material has rare earth europium (Eu)2+) Excited CaAl2O4、SrAl2O4、Sr4Al14O25、SrAl4O7、BaAl2O4The wavelength of the emitted light of the materials is 400nm-530nm, and the afterglow time is about 2000 min.
Through the research of the literature, the Chinese patent application number is 97121964.8, and the publication number is: 1188788, the name is: a luminous storage luminescent material and a preparation method thereof, and the patent discloses that the chemical composition of the aluminate long afterglow luminescent material is MO Al2O3Eu, N, wherein M represents Sr or Ga, and N represents Dy or Sm. The preparation method comprises the steps of weighing oxides of aluminum, strontium, calcium and boron or salts capable of generating the oxides by heating according to the ratio of each element component in the chemical composition formula, adding 1-10% of carbon powder with the same volume, adding 1-10% of boric acid for reducing the reaction temperature, grinding and mixing, filling the mixture into a sealed container, sealing, calcining in a high-temperature furnace at 1420-1600 ℃ for 10 minutes to 6 hoursIn the meantime, the mixture is taken out, cooled and then pulverized. The luminescent powder obtained by the process has thicker particles, generally more than 10 microns, and cannot be used in certain occasions with higher requirements on fineness. For example, in the printing industry, luminescent inks can be used to print advertising posters and posters to achieve certain effects at night. However, the particle size of the powder material used in the ink must be in the nanometer scale, and the printing quality can be guaranteed. Luminescent materials have not found application in these industries due to the size limitations of the luminescent powder particles.
Disclosure of Invention
The invention provides a nano aluminate long afterglow luminescent material and a preparation method thereof, aiming at the defects of the prior art, and the nano aluminate long afterglow luminescent material is prepared by utilizing a nano synthesis technology, so that the problem of large and thick particles of the existing long afterglow luminescent powder is solved, and the application field of the long afterglow luminescent material is greatly expanded.
The invention is realized by the following technical scheme. The chemical composition of the nano aluminate long afterglow luminescent material is represented by the following general formula:
xMO·yAl2O3:Eu0.01x，Dy0.02x
wherein, M is Sr or Ca, x is 1, y is 1 or x is 4, and y is 7.
The material is a nano afterglow luminescent material which takes aluminate as a matrix, co-excited ions which can generate traps in crystal lattices by rare earth ions, Dy and the like as an activator and improves afterglow performance by adding a boron-containing compound.
The nano aluminate long afterglow luminescent material is prepared through coprecipitation process with Sr (NO)3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2O、(NH4)2CO3、Eu2O3、Dy2O3、H3BO3、HNO3As raw materials, Eu2O3、Dy2O3Dissolved in HNO3In the presence of a trivalent nitrate solution, Sr (NO)3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2Dissolving O in deionized water to form nitrate solution, weighing the above nitrate solution according to molar ratio in chemical formula, mixing well, and adding (NH)4)2CO3The solutionwas precipitated according to the following equation:
at the same time, the nitrate of rare earth is also simultaneously reacted with (NH)4)2CO3React and precipitate at the same time. The precipitated product is a mixture of substances with good homogeneity and very small particle size. Washing the precipitate thoroughly, drying, adding H3BO3Taking out after ball milling, fully drying, and calcining at high temperature in weak reducing atmosphere to obtain the nano luminescent powder with long afterglow effect.
The method of the present invention is further described below, with the following specific steps:
(1) and (4) solution preparation. The raw material adopts chemically pure Sr (NO)3)2，Ca(NO3)2·6H2O，Al(NO3)3·9H2O，(NH4)2CO3，Eu2O3，Dy2O3，H3BO3，HNO3. Respectively weighing Eu2O3、Dy2O3And placed in a beaker. Measuring concentrated nitric acid HNO3Density 1.46, specific gravity 68% were added to each of the two beakers. Adding deionized water, transferring into volumetric flask after reaction is completed and rare earth oxide is completely dissolved, adding deionized water to 1000ml to obtain 0.1M Eu (NO)3)3And 0.1M Dy (NO)3)3And (3) solution.Weighing Sr (NO)3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2O、(NH4)2CO3The solutions were dissolved in 500ml of deionized water, and after the solutions were completely dissolved, the solutions were adjusted to 1000ml to obtain 1M solutions of the above-mentioned respective substances.
(2) And (4) coprecipitation. Respectively weighing the above nitrate solutions according to different compositions, mixing thoroughly, and using (NH)4)2CO3The solution is subjected to coprecipitation. After the precipitation was completed, it was allowed to stand for 4 hours.
(3) And (6) treating the precipitate. And (4) performing suction filtration by using a vacuum suction filter to separate liquid from solid. And washing and filtering the obtained precipitate with water to remove residual ions. Drying in an oven at 90 ℃.
(4) And (5) ball milling and mixing. Weighing H with 1-3% of precipitate by weight3BO3Mixing with dried precipitate, adding into ball mill, adding 40ml anhydrous alcohol, ball milling for 2 hr, taking out, and drying at 90 deg.C.
(5) And (4) synthesizing. The synthesis was performed using a weakly reducing atmosphere. Carbon powder is used as a reducing agent, the mixture is made into a closed carbon tank, the mixture is filled into the closed carbon tank for sealing, and the sealed carbon tank is placed into a closed alumina crucible. Then burning for 2-4 hours in a high temperature furnace at 1100-1300 ℃, taking out and cooling, and sieving to obtain the aluminate long afterglow luminescent nano powder.
The nano long afterglow luminescent material has CaO and Al in different color tones2O3:Eu0.01，Dy0.02Is bluish purple, SrO. Al2O3:Eu0.01，Dy0.02Is yellow-green, 4 SrO.7Al2O3:Eu0.04，Dy0.08Is blue-green. The obtained nano-scale powder has good dispersibility, can be mixed into printing ink and paint, and can be formed into printed matters, lamp box advertisement pictures and the like with a certain luminous effect by means of screen printing, offset printing or spray painting, and the function is only possessed by nano-scale materials,has afterglow luminescence function in dark environment.
Detailed Description
The following examples are provided in connection with the present disclosure and are set forth to further illustrate the invention.
Example 1, MO was CaO, x was 1, y was 1, and the obtained material was CaO · Al2O3:Eu0.01，Dy0.02Long persistence luminescent materials.
Measuring 1M Ca (NO)3)2Solution 100ml, 1M Al (NO)3)3Solution 200ml, 0.1M Eu (NO)3)310ml of solution, 0.1M Dy (NO)3)320ml of the solution was mixed well and stirred. Separately, 1M (NH) was measured4)2CO3404.5ml of the solution was slowly dropped into the above nitrate mixed solution. After the precipitation is finished, standing for 4 hours, and carrying out vacuum filtration. The obtained precipitate was washed with water and filtered repeatedly for 3 times, and then sufficiently dried at 90 ℃.
Taking 20 g of the dried precipitate, adding 1% of H3BO3. Placing the mixture into an alumina ball milling tank, taking out the mixture after ball milling for 2 hours, and fully drying the mixture at 90 ℃.
The synthesis was performed using a weakly reducing atmosphere. Using carbon powder as reducing agent, making it into closed carbon tank, and making the above-mentioned materialThe mixture was sealed in a sealed carbon canister and placed in a sealed alumina crucible. Calcining in an electric furnace at 1150 deg.C for 2 hr, cooling, taking out, and sieving to obtain CaO-Al2O3:Eu0.01，Dy0.02Long persistence luminescent materials.
The example material appeared white in appearance. XRD test shows that the structure is monoclinic phosphoquartz type structure and the phase composition is CaAl2O4. After being irradiated by sunlight or ultraviolet rays, the purple light afterglow glows in a dark place; when the light source is removed, the material can distinguish the luminous brightness (0.32 mcd/m) in human eyes2) The above can also emit light for 6 hours or more. The example materials were subjected to spectroscopic measurements with an emission wavelength of 436nmTo (3). The average particle diameter of the powder is 70-80nm by field emission electron microscope observation.
Example 2 MO was SrO, x ═ 1, y ═ 1, and the material obtained was SrO · Al2O3:Eu0.01，Dy0.02Long persistence luminescent materials.
Measuring 1M Sr (NO)3)2Solution 100ml, 1M Al (NO)3)3Solution 200ml, 0.1M Eu (NO)3)310ml of solution, 0.1M Dy (NO)3)320ml of the solution was mixed well and stirred. Separately, 1M (NH) was measured4)2CO3404.5ml of the solution was slowly dropped into the above nitrate mixed solution. After the precipitation is finished, standing for 4 hours, and carrying out vacuum filtration. The obtained precipitate was washed with water and filtered repeatedly for 3 times, and then sufficiently dried at 90 ℃.
Taking 20g of the dried precipitate, adding 3% of H3BO3. Placing the mixture into an alumina ball milling tank, taking out the mixture after ball milling for 2 hours, and fully drying the mixture at 90 ℃.
The synthesis was performed using a weakly reducing atmosphere. Carbon powder is used as a reducing agent, the mixture is made into a closed carbon tank, the mixture is filled into the closed carbon tank for sealing, and the sealed carbon tank is placed into a closed alumina crucible. Calcining in electric furnace at 1200 deg.C for 4 hr, cooling, taking out, and sieving to obtain SrO-Al2O3:Eu0.01，Dy0.02Long persistence luminescent materials.
The example material was light yellow in appearance. XRD test shows that the structure is monoclinic phosphoquartz type structure and the phase composition is SrAl2O4. After being irradiated by sunlight or ultraviolet rays, the yellow-green afterglow glows in a dark place; when the light source is removed, the material can distinguish the luminous brightness (0.32 mcd/m) in human eyes2) The above can also emit light for 10 hours or more. The example material was subjected to spectroscopic testing and its emission wavelength was at 510 nm. The powder is regular spherical and has good dispersibility by observation of a field emission electron microscope. The average particle diameter of the powder is 80-100 nm.
Example 3 with MO SrO, x-4, y-7, and a material of 4 sro.7 Al was obtained2O3:Eu0.04，Dy0.08Long persistence luminescent materials.
Measuring 1M Sr (NO)3)2Solution 40ml, 1M Al (NO)3)3Solution 140ml, 0.1M Eu (NO)3)34ml of solution, 0.1M Dy (NO)3)38ml of the solution was thoroughly mixed and stirred. Separately, 1M(NH) was measured4)2CO3251.8ml of the solution was slowly dropped into the above nitrate mixed solution. Standing for 4 hr after precipitation, and vacuum pumpingAnd (5) filtering. The obtained precipitate was washed with water and filtered repeatedly for 3 times, and then sufficiently dried at 90 ℃.
Taking 20 g of the dried precipitate, adding 2% of H3BO3. Placing the mixture into an alumina ball milling tank, taking out the mixture after ball milling for 2 hours, and fully drying the mixture at 90 ℃.
The synthesis was performed using a weakly reducing atmosphere. Carbon powder is used as a reducing agent, the mixture is made into a closed carbon tank, the mixture is filled into the closed carbon tank for sealing, and the sealed carbon tank is placed into a closed alumina crucible. Calcining in an electric furnace at 1300 ℃ for 2 hours, cooling, taking out, and sieving to obtain 4 SrO7 Al2O3:Eu0.04，Dy0.08Long persistence luminescent materials.
The example material was light green in appearance. XRD test shows that the structure is tetragonal structure and the phase composition is Sr4Al14O25. After being irradiated by sunlight or ultraviolet rays, the LED lamp presents blue-green afterglow luminescence in a dark place; when the light source is removed, the material can distinguish the luminous brightness (0.32 mcd/m) in human eyes2) The above can also emit light for 10 hours or more. The example material was tested spectroscopically and its emission wavelength was at 485 nm. The powder is regular spherical and has good dispersibility through the observation of a field emission electron microscope, and the average particle diameter of the powder is 120-130 nm.
Claims (4)
1. A nano aluminate long afterglow luminescent material is characterized in that the chemical formula is as follows: xMO. yAl2O3：Eu0.01x，Dy0.02x.Wherein, M is Sr or Ca, x is 1, y is 1 or x is 4, and y is 7.
2. The nano aluminate long afterglow luminescent material of claim 1, wherein the nano long afterglow luminescent material is prepared by adding boron-containing compound to aluminate as matrix, rare earth ions and co-excited ions capable of generating traps in crystal lattice as activator.
3. A long-afterglow luminescent nano-aluminate material is prepared from Sr (NO) through coprecipitation3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2O、(NH4)2CO3、Eu2O3、Dy2O3、H3BO3、HNO3As raw materials, Eu2O3，Dy2O3Dissolved in HNO3In the presence of a trivalent nitrate solution, Sr (NO)3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2Dissolving O in deionized water to form nitrate solution, weighing the above nitrate solution according to molar ratio in chemical formula, mixing well, and adding (NH)4)2CO3Precipitating the solution, washing and drying the precipitate, and adding H3BO3Taking out after ball milling, fully drying, and calcining at high temperature in weak reducing atmosphere to obtain the nano aluminate long afterglow luminescent powder.
4. The method for preparing the silicate long-afterglow luminescent material as claimed in claim 3, which is characterized by further limiting the method of the invention as follows:
(1) solution preparation: the raw material adopts chemically pure Sr (NO)3)2，Ca(NO3)2·6H2O，Al(NO3)3·9H2O，(NH4)2CO3，Eu2O3，Dy2O3，H3BO3，HNO3. Respectively weighing Eu2O3、Dy2O3Placing the mixture in a beaker, and measuring concentrated nitric acid HNO3Respectively adding the rare earth oxide with the density of 1.46 and the specific gravity of 68% into two beakers, adding deionized water, transferring into a volumetric flask after the reaction is completed and the rare earth oxide is completely dissolved, adding the deionized water to 1000ml, and obtaining 0.1M Eu (NO)3)3And 0.1M Dy (NO)3)3Solution, weighing Sr (NO)3)2、Ca(NO3)2·6H2O、Al(NO3)3·9H2O、(NH4)2CO3Respectively dissolving in 500ml of deionized water, and adjusting the solution to 1000ml after the deionized water is completely dissolved to obtain 1M solution of the above substances;
(2) coprecipitation: measuring the above nitrate solutions according to the composition, mixing well, and using (NH)4)2CO3Coprecipitating the solution, and standing for 4 hours after the precipitation is finished;
(3) and (3) treating precipitates: performing suction filtration by using a vacuum suction filter, separating liquid from solid, washing and suction-filtering the obtained precipitate with water, removing residual ions, and drying in a drying oven at 90 ℃;
(4) ball milling and mixing: weighing H with 1-3% of precipitate by weight3BO3Mixing with the dried precipitate, adding into a ball mill, adding 40ml of anhydrous ethanol, ball milling for 2 hours, taking out, and fully drying at 90 ℃;
(5) synthesizing: synthesizing by using weak reducing atmosphere, using carbon powder as a reducing agent, making the reducing agent into a closed carbon tank, putting the mixture into the closed carbon tank, sealing, putting the sealed carbon tank into a closed alumina crucible, then burning the mixture for 2 to 4 hours in a high-temperature furnace at 1100 to 1300 ℃, taking out the mixture, cooling and sieving the mixture to obtain the aluminate long-afterglow luminescent nano-powder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432184C (en) * | 2005-03-25 | 2008-11-12 | 上海师范大学 | Preparation of visible light -initiated nano superlong-persistence luminescent materials |
| CN100457852C (en) * | 2005-06-16 | 2009-02-04 | 中国科学院合肥物质科学研究院 | Nanotube, nano bar-shape aluminate long afterglow materials and method for preparing same |
| CN100497518C (en) * | 2006-04-27 | 2009-06-10 | 昆明贵金属研究所 | Process for preparing aluminate luminescent materials |
| CN101319376B (en) * | 2007-06-06 | 2012-06-13 | 中国科学院金属研究所 | Rare earth doping nano SrAl2O4 material and method for producing the same |
| CN102703068A (en) * | 2012-05-18 | 2012-10-03 | 暨南大学 | High-brightness nano strontium-aluminate long-afterglow luminous material and preparation method and application thereof |
| CN106947470A (en) * | 2017-03-31 | 2017-07-14 | 英特美光电（苏州）有限公司 | LED and remote fluorescence device small size salt a kind of novel processing step |
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2004
- 2004-04-08 CN CN 200410017536 patent/CN1246419C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432184C (en) * | 2005-03-25 | 2008-11-12 | 上海师范大学 | Preparation of visible light -initiated nano superlong-persistence luminescent materials |
| CN100457852C (en) * | 2005-06-16 | 2009-02-04 | 中国科学院合肥物质科学研究院 | Nanotube, nano bar-shape aluminate long afterglow materials and method for preparing same |
| CN100497518C (en) * | 2006-04-27 | 2009-06-10 | 昆明贵金属研究所 | Process for preparing aluminate luminescent materials |
| CN101319376B (en) * | 2007-06-06 | 2012-06-13 | 中国科学院金属研究所 | Rare earth doping nano SrAl2O4 material and method for producing the same |
| CN102703068A (en) * | 2012-05-18 | 2012-10-03 | 暨南大学 | High-brightness nano strontium-aluminate long-afterglow luminous material and preparation method and application thereof |
| CN106947470A (en) * | 2017-03-31 | 2017-07-14 | 英特美光电（苏州）有限公司 | LED and remote fluorescence device small size salt a kind of novel processing step |
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