Method for preparing high-luminous-intensity water-resistant phosphor powder

[0023] Example 1

[0024] Mix water glass and silicon dioxide at a mass ratio of 3:1 and stir for 8 minutes to obtain a mixture. Mix the mixture, deionized water and sesame oil in a flask at a mass ratio of 5:3:1 and stir for 10 minutes. After stirring, The flask was placed in an ultrasonic disperser for ultrasonic dispersion for 20 minutes, and after dispersion, it was heated and refluxed at a temperature of 85°C for 1 hour to obtain a reaction solution, which was washed with absolute ethanol for 3 times, air-dried naturally, ground and discharged to obtain a self-made mixture; Add 80mL of hydrofluoric acid solution with a mass fraction of 42% and 60mL of deionized water into a polyethylene beaker, mix and stir for 10min, then place in an ice-water bath at 0°C to cool for 20min, then continue to add 45g of carbonic acid to the polyethylene beaker after cooling Magnesium, mixed and stirred for 1h, filtered to remove the filtrate, put the filter residue in a kiln, and dried at a temperature of 300°C for 2h to obtain self-made magnesium fluoride; weigh 16g of yttrium nitrate and 4g of europium nitrate and mix them in a 100mL deionized Stir in a beaker of water for 16 min to obtain a self-made solution, then add 0.6 g of ammonium metavanadate and 1 g of disodium edetate to the self-made solution, continue stirring for 20 min to obtain a modified solution, and use 24% nitric acid The solution adjusts the pH of the modified solution to 1; in parts by weight, weigh 20 parts of the modified solution, 10 parts of the self-made mixture, 6 parts of the self-made magnesium fluoride and 3 parts of polytetrafluoroethylene and mix them in the reaction kettle to stir the reaction After 20 minutes, heat up to 160°C, then add 2 parts of polyvinylpyrrolidone and 1 part of sodium lauryl sulfate, continue to insulate and stir for 1 hour, cool naturally to room temperature to obtain a suspension, wash the suspension twice with absolute ethanol, Centrifuge and stand still, separate and remove the water phase, and finally put it into an oven, dry at a temperature of 75°C for 3 hours, cool down, grind and discharge, and then the water-resistant phosphor with high luminous intensity can be prepared.

[0025] Example 2

[0026]Mix water glass and silicon dioxide at a mass ratio of 3:1 and stir for 9 minutes to obtain a mixture. Mix the mixture, deionized water and sesame oil at a mass ratio of 5:3:1 and place them in a flask and stir for 11 minutes. After stirring, The flask was placed in an ultrasonic dispersing machine for ultrasonic dispersion for 25 minutes. After dispersion, it was heated and refluxed at a temperature of 87°C for 2 hours to obtain a reaction solution. The reaction solution was washed with absolute ethanol for 4 times, air-dried naturally, and ground and discharged to obtain a self-made mixture; Add 90mL of hydrofluoric acid solution with a mass fraction of 42% and 70mL of deionized water to a polyethylene beaker, mix and stir for 11min, and then cool in an ice-water bath at 0°C for 25min, then continue to add 50g of carbonic acid to the polyethylene beaker after cooling. Magnesium, mixed and stirred for 1.5h, filtered to remove the filtrate, put the filter residue in a kiln, and dried at a temperature of 350°C for 3h to obtain self-made magnesium fluoride; weigh 18g of yttrium nitrate and 5g of europium nitrate and mix them in a 110mL Stir in a beaker of ionized water for 18min to obtain a self-made solution, then add 0.7g ammonium metavanadate and 1g disodium edetate to the self-made solution, and continue stirring for 25min to obtain a modified solution. Adjust the pH of the modified solution to 1 with nitric acid solution; weigh 25 parts of the modified solution, 11 parts of the self-made mixture, 7 parts of the self-made magnesium fluoride and 4 parts of polytetrafluoroethylene, mix them in the reaction kettle and stir React for 25 minutes, heat up to 170°C, add 3 parts of polyvinylpyrrolidone and 2 parts of sodium lauryl sulfate, continue to keep warm and stir for 1.5 hours, cool naturally to room temperature to obtain a suspension, wash the suspension with absolute ethanol for 3 The second time, centrifuge and stand still, separate and remove the water phase, and finally put it into an oven, dry at 80°C for 4 hours, cool down, grind and discharge, and then the water-resistant phosphor with high luminous intensity can be prepared.

[0027] Example 3

[0028] Mix water glass and silicon dioxide at a mass ratio of 3:1 and stir for 10 minutes to obtain a mixture. Mix the mixture, deionized water and sesame oil at a mass ratio of 5:3:1 and place them in a flask and stir for 12 minutes. After stirring, The flask was placed in an ultrasonic disperser for ultrasonic dispersion for 30 minutes, and then heated and refluxed at a temperature of 90° C. for 3 hours to obtain a reaction solution. The reaction solution was washed with absolute ethanol for 5 times, air-dried naturally, and ground and discharged to obtain a self-made mixture; Add 100mL of hydrofluoric acid solution with a mass fraction of 42% and 80mL of deionized water to a polyethylene beaker, mix and stir for 12min, then place in an ice-water bath at 0°C to cool for 30min, then continue to add 55g of carbonic acid to the polyethylene beaker after cooling Magnesium, mixed and stirred for 2 hours, filtered to remove the filtrate, put the filter residue in a kiln, and dried at a temperature of 400°C for 4 hours to obtain self-made magnesium fluoride; weigh 20g of yttrium nitrate and 6g of europium nitrate and mix them in a 120mL deionized Stir in a beaker of water for 20 minutes to obtain a self-made solution, then add 0.8 g of ammonium metavanadate and 2 g of disodium edetate to the self-made solution, and continue stirring for 30 minutes to obtain a modified solution. The solution adjusts the pH of the modified solution to 2; in parts by weight, weigh 30 parts of the modified solution, 12 parts of the self-made mixture, 8 parts of the self-made magnesium fluoride and 5 parts of polytetrafluoroethylene and mix them in the reactor to stir the reaction After 30 minutes, heat up to 180°C, then add 4 parts of polyvinylpyrrolidone and 3 parts of sodium lauryl sulfate, continue to keep warm and stir for 2 hours, and naturally cool to room temperature to obtain a suspension, which is washed 4 times with absolute ethanol. Centrifuge and stand still, separate and remove the water phase, and finally put it into an oven, dry at 85°C for 5 hours, cool down, grind and discharge, and then the water-resistant phosphor with high luminous intensity can be prepared.