CN115074128A - Bubble method preparation process of layered nano BAM fluorescent powder - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- 230000003647 oxidation Effects 0.000 claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 20
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 20
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 17
- -1 europium ions Chemical class 0.000 claims abstract description 14
- 229910001422 barium ion Inorganic materials 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 5
- XDFCIPNJCBUZJN-UHFFFAOYSA-N barium(2+) Chemical compound [Ba+2] XDFCIPNJCBUZJN-UHFFFAOYSA-N 0.000 claims abstract description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 description 12
- 239000000203 mixture Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7729—Chalcogenides
- C09K11/7731—Chalcogenides with alkaline earth metals
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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- Engineering & Computer Science (AREA)
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Abstract
The invention provides a bubble method preparation process of layered nanometer BAM fluorescent powder, which adopts a cuboid magnetic boat to replace an original beaker container, then introduces citric acid and polyacrylic acid, forms bubbles in the process of constant temperature stirring, the bubbles form the layered nanometer BAM fluorescent powder at an oxidation temperature, the molecular general formula of the BAM fluorescent powder is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ion Eu2+ to substituted barium ion Ba2+, x is more than or equal to 0.01 and less than or equal to 0.1, the set range of the oxidation temperature is more than or equal to 700 ℃ and less than or equal to 800 ℃, and polyacrylic acid with the temperature of 1 and less than or equal to n: the citric acid is less than or equal to 3. The bubble method preparation process of the layered nano BAM fluorescent powder solves the problem that europium ions may agglomerate when the BAM fluorescent powder is prepared in the prior art.
Description
Technical Field
The invention relates to the field of preparation processes of nano materials, in particular to a bubble method preparation process of layered nano BAM fluorescent powder.
Background
The fluorescent powder is generally divided into light-induced energy storage luminous powder and luminous powder with radioactivity, wherein the light-induced energy storage luminous powder is characterized in that the fluorescent powder stores light energy after being irradiated by natural light, sunlight light, ultraviolet light and the like, and slowly releases the light energy in a fluorescent mode after the light irradiation is stopped, so that the fluorescent powder can still see luminescence at night or in dark places for a lasting time of several hours to more than ten hours.
When the BAM fluorescent powder is prepared, europium ions may have an agglomeration phenomenon, and the problems such as a coprecipitation method and a sol-gel method cannot be solved.
Therefore, it is necessary to provide a bubble method for preparing the layered nano BAM phosphor to solve the above technical problems.
Disclosure of Invention
The invention provides a bubble method preparation process of layered nano BAM fluorescent powder, which solves the problem that europium ions may agglomerate when the BAM fluorescent powder is prepared in the prior art.
In order to solve the technical problems, the bubble method preparation process of the layered nano BAM fluorescent powder provided by the invention adopts a cuboid magnetic boat to replace the original beaker container, then introduces citric acid and polyacrylic acid, forms bubbles in the process of constant-temperature stirring, and forms the layered nano BAM fluorescent powder at an oxidation temperature, wherein the molecular general formula of the BAM fluorescent powder is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ion Eu2+ to barium ion Ba2+, x is more than or equal to 0.01 and less than or equal to 0.1, the set range of the oxidation temperature is more than or equal to 700 ℃ and less than or equal to 800 ℃, and polyacrylic acid is more than or equal to 1: the citric acid is less than or equal to 3.
The preparation steps of the BAM fluorescent powder are as follows;
step A, firstly determining the stoichiometric ratio of each element in Ba1-xEuxMgAl10O17, and weighing each component raw material by taking 0.0001mol as a unit variable;
step B, pouring the raw materials required by the BAM substrate into a beaker A of 200ml, adding 50ml of distilled water, stirring for 30min by using a glass rod, then stirring for 30min at normal temperature of 150r/min on a constant-temperature magnetic stirrer at normal temperature, pouring citric acid into a beaker B of 100ml, adding 50ml of distilled water, and stirring until the water is clear;
step C, pouring the solution in the beaker B into the beaker A to obtain clear mixed liquid, keeping the temperature at 50 ℃, stirring for 1h at 300r/min, then adding polyacrylic acid into the beaker A, and continuing stirring at the original speed until the solution is clear, colorless and transparent;
and D, adding 0.5mol of ethylene glycol, and detecting the pH value by using a pH test paper to be in a range of 9-10.
Step E, pouring the mixed solution in the beaker A into a cooled and disinfected magnetic boat, adjusting the temperature of a constant-temperature stirrer to be 50-100 ℃, and increasing a temperature gradient of 10 ℃ to about 100 ℃ from 50 ℃ every ten minutes;
and step F, turning off the stirrer, quickly putting the magnetic boat into an oxidation muffle furnace by using tweezers, after the oxidation time of 700 ℃ for 3 hours, putting the magnetic boat into a test tube furnace of 95% N2 and 5% H2 for 1300 ℃ for 4 hours, and taking out the magnetic boat to obtain the special layered nano BAM fluorescent powder.
Preferably, the raw materials are Ba (NO3)2 of 0.0261X (0.99X 0.9) g, Mg (NO3) 2.6H 2O of 0.0256g, Al (NO3) 3.9H 2O of 0.375g, Eu (NO3) 3.6H 2O of 0.0446(1-X) g, ethylene glycol of 0.5mol, polyacrylic acid of 2.4g and citric acid of 0.2522 g.
Preferably, the Ba (NO3)2 is 0.0261X, wherein X is selected to control the content of Eu2+, so as to obtain BAM phosphor with optimal concentration of europium ions, and the values of X are 0.99, 0.97, 0.95, 0.93, and 0.9, respectively, so that the concentration of europium ions varies by 1%, 3%, 5%, 7%, and 10%. Thereby obtaining the BAM fluorescent powder under the optimal europium ion concentration, and obtaining the BAM with the smallest nanometer size of about 270nm under the condition that the europium ion concentration is 1 percent, wherein the BAM with larger size is larger when the europium ion concentration is larger.
Preferably, after the europium ion concentration is determined, the oxidation temperature needs to be adjusted, the temperature is set in three temperature ranges of 700 ℃, 750 ℃ and 800 ℃, and the size of the BAM fluorescent powder is optimal at 700 ℃ and is about 420 nm.
Preferably, after the proportion of polyacrylic acid to citric acid is regulated after the europium ion concentration is 1% and the oxidation temperature is 700 ℃, three intervals of 2:2, 2.5:1.5 and 3:1 are set, and the size of BAM is optimally between 200nm and 450nm when the ratio is 2.5: 1.5.
Compared with the related technology, the bubble method preparation process of the layered nano BAM fluorescent powder provided by the invention has the following beneficial effects:
(1) the invention provides a bubble method preparation process of layered nano BAM fluorescent powder, which is characterized in that polyacrylic acid is introduced to generate an electric double layer effect, so that charges with the same polarity are mutually repelled, mixed ions in BAM can generate a good dispersion effect, and in addition, citric acid can surround each ion and polyacrylic acid to form pressure difference, so that bubbles are formed.
(2) The invention provides a bubble method preparation process of layered nano BAM fluorescent powder, which can realize the effect of the layered nano fluorescent powder by introducing the proportion of polyacrylic acid and citric acid, and simultaneously, the best foaming effect can be achieved by replacing the original tool beaker used for reaction with a magnetic boat, and in addition, the oxidation temperature is reduced by 200 plus one-step over 300 ℃ compared with the traditional process, thereby greatly reducing the reaction time.
Drawings
FIG. 1 is a flow chart of a bubble method preparation process of the layered nano BAM fluorescent powder provided by the invention.
Detailed Description
The invention is further described with reference to the following figures and embodiments.
Referring to fig. 1, fig. 1 is a flow chart of a bubble method for preparing a layered nano BAM phosphor, wherein a rectangular magnetic boat is used to replace the original beaker container, and then citric acid and polyacrylic acid are introduced to form bubbles during constant temperature stirring, and the bubbles form the layered nano BAM phosphor at an oxidation temperature, and the method comprises the steps of firstly determining the stoichiometric ratio of each element in Ba 1-xexmgal 10O17, taking 0.0001mol as a unit variable, weighing Ba (NO3)2 as 0.0261X (0.99X ≤ 0.9) g, Mg (NO3) 2.6H 2O as 0.0256g, Al (NO3) 3.9H 2O as 0.375g, Eu (NO3) 3.6H 2O as 0.0446(1-X) g, ethylene glycol as 0.5mol, polyacrylic acid as 2.4g, citric acid as 0. 0.2522g, pouring the raw material into a beaker for stirring, adding 30 ml of distilled water into a beaker, and stirring the raw material as 50ml, then placing the mixture on a constant-temperature magnetic stirrer, stirring the mixture for 30min at the normal temperature of 150r/min, then pouring citric acid into a 100ml beaker B, adding 50ml of distilled water, stirring the mixture until the water is clear, pouring the solution in the beaker B into the beaker A to obtain a clear mixed liquid, keeping the temperature of 50 ℃, stirring the mixture for 1H at the speed of 300r/min, then pouring polyacrylic acid into the beaker A, stirring the mixture at the original speed until the solution is clear, colorless and transparent, adding 0.5mol of ethylene glycol, detecting the pH test paper to be in a range of between 9 and 10, pouring the mixed solution in the beaker A into a cooled and sterilized magnetic boat, simultaneously adjusting the temperature of the constant-temperature stirrer to be between 50 and 100 ℃, adding a temperature gradient of 10 ℃ from 50 ℃ to about 100 ℃ every ten minutes, turning off the stirrer, rapidly placing the magnetic boat into an oxidation muffle furnace by using special forceps, and taking the magnetic boat out the magnetic boat after the oxidation time of 700 ℃ is 3H, and then placing the magnetic boat into a test tube furnace with the temperature of 95% N2 and 5% H2 for 1300 ℃ to obtain an oxidation time of 4H The nano BAM fluorescent powder is in a shape of a sphere.
The embodiment of the bubble method preparation process of the layered nano BAM fluorescent powder provided by the invention is as follows:
example 1: preparation of Ba0.99Eu0.01MgAl10O17 fluorescent powder
According to the stoichiometric ratio of each element in the chemical formula Ba0.99Eu0.01MgAl10O17, 0.258g of Ba (NO3)2(A.R), 0.256g of Mg (NO3) 2.6H 2O (A.R), 3.75g of Al (NO3) 3.9H 2O (4N) and 0.0045g of Eu (NO3) 3.6H 2O (4N) are accurately weighed, 200ml of distilled water is filled in a beaker A of the mixed ionic solution, the beaker A is stirred for half H by a glass rod, the beaker is placed on a stirrer and stirred for 1H, then C6H8O7(A.R)2.522g and 24g of polyacrylic acid (A.R) are weighed and placed in a beaker B of 200ml of distilled water, and the beaker is stirred to be transparent by the same method. Mixing the solution in the beaker A and the solution in the beaker B, putting the mixture in a big beaker, adding 5 ml of ethylene glycol, stirring for 10-20min, and detecting the mixture in a range of 9-10 by using a pH test paper. At this point the mixture was transferred to a magnetic boat and the temperature of the thermostatic magnetic stirrer was controlled to accelerate from 50 ℃ to 100 ℃ at 10 ℃ per hour until the solution started to foam and the stirrer was quickly removed. The magnetic boat is put into an oxidation muffle furnace for 3 hours at 700 ℃, and then is oxidized for 4 hours at 1400 ℃ in a test tube furnace for 5% H2/95% N2, and the layered nano BAM fluorescent powder can be obtained after being taken out.
Example 2: preparation of Ba0.97Eu0.03MgAl10O17 fluorescent powder
Other conditions were the same as those in example 1 except that "Ba (NO3)2(A.R)0.258 g" in example 1 was changed to "Ba (NO3)2(A.R)0.253 g", and "Eu (NO3) 3.6H 2O (4N)0.0045 g" in example 1 was changed to "Eu (NO3) 3.6H 2O (4N)0.0135 g", thereby obtaining Ba0.97Eu0.03MgAl10O17 blue phosphor.
Example 3: preparation of Ba0.95Eu0.05MgAl10O17 fluorescent powder
Other conditions were the same as those in example 1 except that "Ba (NO3)2(A.R)0.258 g" in example 1 was changed to "Ba (NO3)2(A.R)0.248 g" and "Eu (NO3) 3.6H 2O (4N)0.0045 g" in example 1 was changed to "Eu (NO3) 3.6H 2O (4N)0.0225 g" in example 1, to obtain Ba0.97Eu0.03MgAl10O17 blue phosphor.
Example 4: preparation of Ba0.93Eu0.07MgAl10O17 fluorescent powder
Other conditions were the same as those in example 1 except that "Ba (NO3)2(A.R)0.258 g" in example 1 was changed to "Ba (NO3)2(A.R)0.243 g" and "Eu (NO3) 3.6H 2O (4N)0.0045 g" in example 1 was changed to "Eu (NO3) 3.6H 2O (4N)0.0315 g", respectively, to obtain Ba0.Eu930.07MgAl10O17 blue phosphor.
Example 5: preparation of Ba0.9Eu0.1MgAl10O17 fluorescent powder
Other conditions were the same as those in example 1 except that "Ba (NO3)2(A.R)0.258 g" in example 1 was changed to "Ba (NO3)2(A.R)0.235 g" and "Eu (NO3) 3.6H 2O (4N)0.0045 g" in example 1 was changed to "Eu (NO3) 3.6H 2O (4N)0.045 g", thereby obtaining Ba0.9Eu0.1MgAl10O17 blue phosphor.
Compared with the related technology, the bubble method preparation process of the layered nano BAM fluorescent powder provided by the invention has the following beneficial effects:
the effect of the layered nano fluorescent powder can be realized by introducing the proportion blending of polyacrylic acid and citric acid, meanwhile, the original tool beaker used for reaction is replaced by a magnetic boat, the optimal foaming effect can be achieved, in addition, the oxidation temperature is reduced by 200-300 ℃ compared with the traditional process, the reaction time is greatly reduced, and the problem that europium ions can be agglomerated during the preparation of BAM fluorescent powder in the prior art is solved.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (7)
1. A bubble method for preparing layered nanometer BAM fluorescent powder is characterized in that a cuboid magnetic boat is adopted to replace an original beaker container, citric acid and polyacrylic acid are introduced, bubbles are formed in the process of constant-temperature stirring, and the bubbles form the layered nanometer BAM fluorescent powder at an oxidation temperature.
2. The process of claim 1, wherein the BAM phosphor has a molecular formula of Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ion Eu2+ to barium ion Ba2+, 0.01. ltoreq. x.ltoreq.0.1, the oxidation temperature is set in the range of 700. ltoreq. T.ltoreq.800 ℃, 1. ltoreq. n polyacrylic acid: the citric acid is less than or equal to 3.
3. The bubble method preparation process of layered nano BAM phosphor of claim 2, wherein the BAM phosphor is prepared by the following steps;
step A, firstly determining the stoichiometric ratio of each element in Ba1-xEuxMgAl10O17, and weighing each component raw material by taking 0.0001mol as a unit variable;
step B, pouring the raw materials required by the BAM substrate into a beaker A of 200ml, adding 50ml of distilled water, stirring for 30min by using a glass rod, then placing the beaker on a constant-temperature magnetic stirrer, stirring for 30min at normal temperature of 150r/min, then pouring citric acid into a beaker B of 100ml, adding 50ml of distilled water, and stirring until the water is clear;
step C, pouring the solution in the beaker B into the beaker A to obtain clear mixed liquid, keeping the temperature at 50 ℃, stirring for 1h at 300r/min, then pouring polyacrylic acid into the beaker A, and continuing stirring at the original speed until the solution is clear, colorless and transparent;
and D, adding 0.5mol of ethylene glycol, and detecting the pH value by using a pH test paper to be in a range of 9-10.
Step E, pouring the mixed solution in the beaker A into a cooled and disinfected magnetic boat, adjusting the temperature of a constant-temperature stirrer to be 50-100 ℃, and increasing the temperature from 50 ℃ to 100 ℃ by a temperature gradient of 10 ℃ every ten minutes;
and step F, turning off the stirrer, quickly putting the magnetic boat into an oxidation muffle furnace by using tweezers, after 3 hours of oxidation time at 700 ℃, putting the magnetic boat into a test tube furnace with 95% of N2 and 5% of H2 for 1300 ℃ for 4 hours, and taking out the special layered nano BAM fluorescent powder.
4. The bubble method for preparing layered nanometer BAM phosphor as claimed in claim 3, wherein the raw material in step A is Ba (NO3)2 is 0.0261X (0.99X 0.9), Mg (NO3) 2.6H 2O is 0.0256g, Al (NO3) 3.9H 2O is 0.375g, Eu (NO3) 3.6H 2O is 0.0446(1-X) g, ethylene glycol is 0.5mol, polyacrylic acid is 2.4g, citric acid is 0.2522 g.
5. The bubble method of claim 4, wherein Ba (NO3)2 is 0.0261X, X is 0.99, 0.97, 0.95, 0.93, 0.9, and concentration of europium ion is 1%, 3%, 5%, 7%, 10%.
6. The bubble process of claim 5, wherein the europium ion concentration is determined and the oxidation temperature is adjusted to be within three temperature ranges of 700 ℃, 750 ℃ and 800 ℃.
7. The bubble method preparation process of claim 6, wherein after the europium ion concentration is 1% and the oxidation temperature is 700 ℃, the ratio of polyacrylic acid to citric acid is adjusted to set three intervals as 2:2, 2.5:1.5 and 3:1, respectively.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109897635A (en) * | 2019-04-26 | 2019-06-18 | 重庆三峡学院 | A kind of preparation method of space lighting systems aluminate luminescent material |
| CN111187532A (en) * | 2019-11-27 | 2020-05-22 | 甘肃稀土新材料股份有限公司 | BAM-based automobile paint with fluorescent whitening effect and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109897635A (en) * | 2019-04-26 | 2019-06-18 | 重庆三峡学院 | A kind of preparation method of space lighting systems aluminate luminescent material |
| CN111187532A (en) * | 2019-11-27 | 2020-05-22 | 甘肃稀土新材料股份有限公司 | BAM-based automobile paint with fluorescent whitening effect and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 李鸣: ""钇铝石榴石粉体的低温合成及YAG透明陶瓷的快速制备"", 《中国优秀硕士论文全文数据库 工程科技Ⅰ辑》 * |
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