CN1307082A - Method for preparing long aftergrow inorganic luminous material - Google Patents

Method for preparing long aftergrow inorganic luminous material Download PDF

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Publication number
CN1307082A
CN1307082A CN 00100321 CN00100321A CN1307082A CN 1307082 A CN1307082 A CN 1307082A CN 00100321 CN00100321 CN 00100321 CN 00100321 A CN00100321 A CN 00100321A CN 1307082 A CN1307082 A CN 1307082A
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burning
elements selected
luminescent material
light
luminous material
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CN1117134C (en
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张明
霍力
夏仕美
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Sichuan Sunfor Light Co Ltd
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XINLI INDUSTRIAL GROUP Co Ltd SICHUAN
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Abstract

The long afterglow inorganic luminous material has chemical composition of aMO.bN2O3.xRO.yTR2O3, where M is group IIA element, N is group IIIA element, R is selected from Eu, Sm and Yb, TR lanthanides, a is 0.5-5, b is 0.5-7, x is 0.0001-0.5 and y is 0.0001-0.5. Its preparation includes ignition of material in reductive atmosphere and the further treatment of material with silicate solution or methyl silicone oil solution. The product has homogeneous granularity and water resistance.

Description

Preparation method of long afterglow inorganic luminescent material
The invention relates to a preparation method of a long-afterglow phosphor, in particular to a method of a rare earth ion co-activated IIA and IIIA main group element oxide phosphor.
The long-afterglow luminescent material is a material which has energy storage performance after being irradiated by sunlight or other light sources, can emit light for a long time in a dark place, and can store light and emit light repeatedly for many times.
Most of the conventional light-storing and light-emitting materials are sulfide type compounds, such as ZnS: Cu (green light-emitting), CaS: Bi (violet blue light-emitting), or ZnCdS: Cu (yellow-orange light-emitting). However, these sulfides have a short afterglow time, unstable properties, poor light resistance and a short service life. Basically, the afterglow time of the afterglow can not meet the requirement even if the afterglow time is 20 to 30 minutes.
Another phosphorescent phosphor developed in the past contains a radioactive substance. The material can emit light for a long time, but radioactive substances are well-known dangerous pollution sources and can cause serious damage to human bodies and the environment, so that the material is strictly forbidden internationally.
In the early nineties, a light-excited luminescent material with a long afterglow, such as CN1053807A, was developed, which discloses a luminescent material with a long afterglow, having the general formula m (Sr)1-xEux)O·nAl2O3·yB2O3Wherein m is more than or equal to 1 and less than or equal to 5, n is more than or equal to 1 and less than or equal to 8, x is more than or equal to 0.001 and less than or equal to 0.1, and y is more than or equal to 0.001 and less than or equal to 0.35. The long afterglow luminescent material has low brightness and afterglow time.
Further, U.S. Pat. Nos. 5,376,303 and 5,424,006 and Japanese patent application Nos. 8-73845,8-127772 disclose Eu2+The activated long-afterglow fluorescent substance of alkaline earth metal aluminate shows higher brightness and afterglow time. However, the sintering temperature is too high, or the excessive boric acid is introduced to lower the sintering temperature, so that the sintered cake is difficult to break, and the brightness of the powder is greatly reduced. Meanwhile, N is adopted2+H2The mixed gas causes poor operation safety and increases the difficulty of equipment. And the requirement on a heating body is higher due to the overhigh sintering temperature, so that the cost is increased.
In addition, the emission luminance of an aluminate luminescent material is related to the intensity of excitation light, and the stronger the excitation light, the higher the luminance, but the effect on weak light excitation is not ideal. Meanwhile, the aluminate luminescent material is unstable when decomposed by water.
In addition, the synthesis temperature is too high, and the particles of the luminescent powder are coarse, so that the luminescent powder cannot be used for printing. Therefore, it is necessary to manufacture a fine-particle luminescent powder.
The invention aims to overcome the defects of the prior art, improve the process, recombine on the proportion of rare earth, reduce the cost and provide a method for manufacturing a low-cost luminescent material with higher brightness and longer afterglow.
It is another object of the present invention to provide a method for producing a luminescent material that can be rapidly excited under low light.
It is a further object of the present invention to provide a method for making a fine-grained phosphor having both high brightness and afterglow time, which meets the printing requirements.
It is another object of the present invention to provide a method for producing a luminescent material having good water resistance, which satisfies the requirements of aqueous coating materials.
In order to achieve the above object, the present invention provides a method for producing a phosphorescent phosphor having a chemical composition satisfying the following general formula:
aMO·bN2O3·xRO·yTR2O3wherein the content of the first and second substances,
m is one or more elements selected from Sr, Ca, Mg and Zn;
n is one or more elements selected from B, Al, Ga and Sc;
r is one or more elements selected from Eu, Sm and Yb;
TR is one or more elements selected from La, Pr, Y, Nd, Dy, Er, Tm and Ho;
a. b, x and y are mole numbers; and the number of the first and second electrodes,
0.5≤a≤5，
0.5≤b≤7，
0.0001≤x≤0.5，
0.0001. ltoreq. y.ltoreq.0.5, preferably
0.8≤a≤2，
1≤b≤2，
0.01≤x≤0.05，
Y is more than or equal to 0.01 and less than or equal to 0.05, and the method comprises the following steps:
mixing the above oxides or oxalate, carbonate or hydroxide corresponding to the above oxides according to the above ratio, adding deionized water 0.5-1.5 times the volume of the above materials, grinding to below 2 μm, oven drying, and adding H at 1200-1400 deg.C2Or H2And CO burning for 2-5 hours.
In the above method, the raw materials are salts corresponding to oxides of IIA and IIIA elements, such as oxalate and carbonic acidThe salt or the hydroxide thereof is weighed according to the mixture ratio of the components, a mud method is adopted, namely a certain amount of water, such as deionized water with the volume of 0.5-1.5 times of the material volume, is added, is ground, is generally ground to the granularity of less than 2 mu m, and is dried. Then, the desired H is obtained by the following chemical reaction in a high temperature furnace2Or H2+CO：
(ii) a Or
(ii) a Or
Therein, i.e. by feeding NH into the high-temperature furnace3Decomposing the mixture into N under heating2And H2Reducing the gas mixture, or carbon particles, in the atmosphere to CO and H2The mixed gas of (1). In the atmosphere, the mixture is burned for 2-5 hours at 1200-1400 ℃, preferably about 1250 ℃.
In the above-mentioned firing process, preferably add and account for 0.1-1% (weight) of the total amount of material sulphur, its function is to improve the granulometry of the product.
After firing, the material is cooled to about 300 ℃ to obtain the luminescent material with uniform fineness. In order to obtain a luminescent material having excellent water resistance, the surface of the luminescent material obtained by firing is further treated with sodium silicate or potassium silicate having a concentration of 0.1 to 2% by weight, or with methyl silicone oil having a concentration of 0.1 to 2% by weight. The specific method comprises the steps of sieving luminescent powder, adding the luminescent powder into the solution with the volume of more than 1 to 3 times of that of the luminescent powder, stirring, precipitating for 20 minutes to 1 hour, removing the supernatant, taking out the precipitate, drying at 70 to 90 ℃, drying at 150 to 250 ℃, and sieving to obtain the water-resistant luminescent powder.
The method of the present invention can raise the performance of phosphor material with relatively low RE content, and compared with conventional one, the product has raised fineness, weak light exciting effect, lasting afterglow and other indexes and water resisting property.
The present invention will be described in detail below by way of examples, which are not intended to limit the scope of the present invention.
In the examples described below, all reagent specifications were guaranteed to be premium grade pure.
Example 1
(Sr0.9Ca0.1)O·(Al1.8Ga0.2)O30.005EuO·0.005Nd2O3Preparation of (1) taking Al (OH)31.8mol、SrCO30.9mol、CaCO30.1mol、Ga2O30.2mol、Eu2(C2O4)3·10H2O0.005 mol、Nd2(C2O4)30.005mol and H3BO30.08mol, grinding to below 2 mu m by a mud method, drying, adding sulfur powder accounting for 0.5 percent of the weight of the whole material, adding a sample into an electric furnace, introducing ammonia gas, igniting for 3 hours at 125 ℃, and then cooling to 300 ℃ to obtain the luminescent powder. Adding 1% sodium silicate alcohol solution with 2 times volume into a stainless steel container, sieving the luminescent powder with a 200-mesh sieve, adding the luminescent powder into the solution, stirring, precipitating for 30 minutes, removing the supernatant, taking out the precipitate, drying at 80 ℃, drying at 200 ℃, and sieving to obtain the water-resistant luminescent powder. The obtained product has an emission peak at 530nm, and is a yellow-green luminophore. Excited by 200lx light source, and the brightness is reduced to 0.32mcd/m2The time of (2) was 65 hours. The main properties are compared with known products of the same type in Table 1.
Example 2
SrO·(Al1.8Ga0.10Sc0.10)O3·0.005EuO·0.005Tm2O3Preparation of
The procedure of example 1 was repeated, except that the starting material used was Al (OH)31.8 mol、SrCO3 1mol、Ga2(CO3)3 0.05 mol、Sc2(CO3)3 0.05 mol、Eu2(C2O4)3·10H2O 0.005 mol、Tm2(C2O4)3 0005mol and H3BO30.08 mol. The emission peak of the obtained product is 518nm, and the product is a green luminophore. Excited by 200lx light source, and the brightness is reduced to 0.32mcd/m2The time of (2) was 55 hours. The main properties are compared with known products of the same type in Table 1.
TABLE 1 Prepared by the method of U.S. Pat. No. 5,424,006Example 3
(Sr0.8Ca0.2)O·1.75Al2O3·0.005EuO·0.005Nd2O3·0.005Er2O3Preparation of
Taking Al (OH)33.5mol、SrCO30.8mol、CaCO30.2mol、Eu2(C2O4)3·10H2O0.005mol、Nd2(C2O4)30.005mol、H3BO30.08mol and Er2O30.005mol, grinding to below 2 μm by a mud method, drying, adding sulfur powder accounting for 1 percent of the weight of the whole material, adding a sample into an electric furnace, adding 13 g of carbon particles, firing for 2 hours at 1300 ℃, and then cooling to 300 ℃ to obtain the luminescent powder.
Adding 2 times volume of 1% methyl silicone oil ethanol solution into a stainless steel container, sieving luminescent powder with a 200-mesh sieve, adding into the solution, stirring, precipitating for 30 minutes, removing the supernatant, taking out the precipitate, drying at 80 ℃, drying at 200 ℃, and sieving to obtain the water-resistant luminescent powder.
The obtained product has an emission peak at 490nm, and is a blue-light emitter. Excited by 200lx light source, and the brightness is reduced to 0.32mcd/m2The time of (2) was 60 hours. The main properties are compared with known products of the same type in Table 2.
TABLE 2
Performance index Example 3 SrAl4O7:Eu,Dy‡
Luminous brightness Time of light emission Particle size D50 150 60 10～13μm 100 40 More than 30 μm
‡ prepared according to the method of US5,376,303
Example 4
(Ca0.9Sr0.1)(Al1.9Y0.1)O4·0.005EuO·0.005Nd2O3Preparation of
The procedure of example 3 was repeated, except that the starting material used was Al (OH)31.9mol、CaCO30.9mol、SrCO30.1mol、Y2O30.1mol、Eu2(C2O4)3·10H2O0.005mol、Nd2(C2O4)30.005mol and H3BO30.08 mol. The obtained product has emission peak at 440nm, and is blue-violet luminophor. Excited by 200lx light source, and the brightness is reduced to 0.32mcd/m2The time of (2) was 48 hours. The main properties are compared with known products of the same type in Table 3.
TABLE 3
Performance index Example 4 CaAl2O4:Eu,Nd$
Luminous brightness Time of light emission Particle size D50 160 48 10～13μm 100 20 More than 35 μm
$Prepared according to the method of US5,376,303
Examples 5 to 8
Preparation of Water-based paint
Mixing 25% of water-based acrylic resin with solid content, 1% of dispersing agent MS-1 accounting for the total weight, 30% of fluorescent body prepared in examples 1, 2, 3 or 4 and 3% of anti-settling agent M-5 in a high-speed dispersing agent at 1000rpm for 5 minutes to obtain a uniform mixture, and filtering the obtained mixture through a 120-mesh screen to respectively obtain finished products 1-4.
After the obtained finished products 1-4 are respectively stored in water for three months, the luminescence of the fluorophor is not influenced.

Claims (6)

1. A process for preparing rare-earth ion co-activated IIA, IIIA main group element oxide inorganic luminescent material with chemical composition aMO bN2O3·xRO·yTR2O3Wherein the content of the first and second substances,
m is one or more elements selected from Sr, Ca, Mg and Zn:
n is one or more elements selected from B, Al, Ga and Sc;
r is one or more elements selected from Eu, Sm and Yb;
TR is one or more elements selected from La, Pr, Y, Nd, Dy, Er, Tm and Ho; a. b, x and y are mole numbers; and the number of the first and second electrodes,
0.5≤a≤5
0.5≤b≤7
0.0001≤x≤0.5
0.0001. ltoreq. y.ltoreq.0.5 the method comprises:
mixing the above oxides or oxalate, carbonate or hydroxide corresponding to the above oxides according to the above ratio, adding deionized water 0.5-1.5 times of the volume of the above materials, grinding to below 2 μm, oven drying, and adding H at 1200-1400 deg.C2Or H2And CO burning for 2-5 hours.
2. The method of claim 1, wherein said H is2Or H2+ CO is obtained by the reaction in a burning environment as follows:
(ii) a Or
(ii) a Or
C+H2O→H2+CO↑。
3. The method according to claim 1, wherein sulfur is added in an amount of 0.1 to 1 wt% based on the total amount of the material during said burning.
4. The method of claim 1, wherein a, b, x, and y are respectively:
0.8≤a≤2，
1≤b≤2，
0.01≤x≤0.05，
0.01≤y≤0.05。
5. the method according to claim 1, further comprising treating the surface of the luminous material obtained by burning with sodium or potassium silicate having a concentration of 0.1 to 2% by weight.
6. The method according to claim 1, further comprising treating the surface of the luminescent material obtained by burning with a methyl silicone oil having a concentration of 0.1 to 2% by weight.
CN 00100321 2000-01-25 2000-01-25 Method for preparing long aftergrow inorganic luminous material Expired - Lifetime CN1117134C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007003102A1 (en) 2005-07-01 2007-01-11 Sichuan Sunfor Light Co. Ltd Long afterglow luminescent material with compounded substrates and its preparation method
CN1301308C (en) * 2004-01-16 2007-02-21 北京有色金属研究总院 High luminosity aluminate long luminous material and preparation process thereof
CN101429432B (en) * 2008-12-12 2011-11-16 江苏博睿光电有限公司 Superfine grain size high light efficiency long afterglow fluorescent powder and its production method
CN109652011A (en) * 2019-01-21 2019-04-19 广东工业大学 Ultraviolet-near infrared absorption material of one kind and the preparation method and application thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1301308C (en) * 2004-01-16 2007-02-21 北京有色金属研究总院 High luminosity aluminate long luminous material and preparation process thereof
WO2007003102A1 (en) 2005-07-01 2007-01-11 Sichuan Sunfor Light Co. Ltd Long afterglow luminescent material with compounded substrates and its preparation method
EP1900789A4 (en) * 2005-07-01 2009-09-09 Sichuan Sunfor Light Co Ltd Long afterglow luminescent material with compounded substrates and its preparation method
US7955523B2 (en) 2005-07-01 2011-06-07 Sichuan Sunfor Light Co., Ltd. Long afterglow luminescent material with compounded substrates and its preparation method
CN101429432B (en) * 2008-12-12 2011-11-16 江苏博睿光电有限公司 Superfine grain size high light efficiency long afterglow fluorescent powder and its production method
CN109652011A (en) * 2019-01-21 2019-04-19 广东工业大学 Ultraviolet-near infrared absorption material of one kind and the preparation method and application thereof

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