CN115074128B - 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 50
- 238000000034 method Methods 0.000 title claims abstract description 27
- 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 51
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 19
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 19
- 230000003647 oxidation Effects 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 18
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 17
- 229910001422 barium ion Inorganic materials 0.000 claims abstract description 5
- 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 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229910020068 MgAl Inorganic materials 0.000 claims 2
- 229910002538 Eu(NO3)3·6H2O Inorganic materials 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- -1 europium ions Chemical class 0.000 abstract description 12
- 150000002500 ions Chemical class 0.000 abstract description 5
- XDFCIPNJCBUZJN-UHFFFAOYSA-N barium(2+) Chemical compound [Ba+2] XDFCIPNJCBUZJN-UHFFFAOYSA-N 0.000 abstract description 2
- 235000015165 citric acid Nutrition 0.000 description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides a bubble method preparation process of layered nano 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, and forms the layered nano BAM fluorescent powder at the oxidation temperature, wherein the molecular general formula of the BAM fluorescent powder is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ions Eu2+ to barium ions Ba2+, x is more than or equal to 0.01 and less than or equal to 0.1, the oxidation temperature setting range is more than or equal to 700 ℃ and less than or equal to 800 ℃, and n polyacrylic acid is more than or equal to 1: 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 are likely to be agglomerated when the BAM fluorescent powder is prepared in the prior art.
Description
Technical Field
The invention relates to the field of a preparation process of nano materials, in particular to a bubble method preparation process of layered nano BAM fluorescent powder.
Background
The fluorescent powder is generally classified into a photoinduced energy-storage luminous powder and a luminous powder with radioactivity, wherein the photoinduced 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 fluorescence mode after stopping the irradiation of the light, so that the luminous powder can still be seen at night or in dark places, and the duration of the luminous powder is as long as several hours to tens of hours.
In the preparation of BAM fluorescent powder, europium ions may have agglomeration phenomenon, such as coprecipitation method and sol-gel method, which cannot solve the problems.
Therefore, there is a need to provide a bubble method process for preparing layered nano-BAM phosphor powder 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 have agglomeration phenomenon when preparing the BAM fluorescent powder in the prior art.
In order to solve the technical problems, the preparation process of the layered nano BAM fluorescent powder by a bubble method adopts a cuboid magnetic boat to replace an original beaker container, then citric acid and polyacrylic acid are introduced, bubbles are formed in the process of constant-temperature stirring, the bubbles form the layered nano BAM fluorescent powder at the oxidation temperature, the molecular general formula of the BAM fluorescent powder is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ions Eu2+ to barium ions Ba2+, x is more than or equal to 0.01 and less than or equal to 0.1, the oxidation temperature setting range is more than or equal to 700 ℃ and less than or equal to 800 ℃, and n polyacrylic acid is more than or equal to 1: citric acid is less than or equal to 3.
The preparation method of the BAM fluorescent powder comprises the following steps of;
step A, firstly determining the stoichiometric ratio of each element in Ba1-xEuxMgAl10O17, and weighing raw materials of each component by taking 0.0001mol as a unit variable;
pouring raw materials required by the BAM matrix into a 200ml beaker A, adding 50ml distilled water, stirring for 30min by using a glass rod, stirring for 30min at the normal temperature of 150r/min on a constant-temperature magnetic stirrer, pouring citric acid into a 100ml beaker B, and adding 50ml distilled water, and stirring until the water is clear;
pouring the solution in the beaker B into the beaker A to obtain clear mixed liquid, keeping the temperature at 50 ℃ and stirring for 1h at 300r/min, adding polyacrylic acid into the beaker A, and continuing stirring at the original speed until the solution is clear, colorless and transparent;
and D, after 0.5mol of ethylene glycol is added, detecting the pH test paper to be in a range of 9-10.
E, pouring the mixed solution of the beaker A into a cooled and sterilized magnetic boat, and simultaneously adjusting the temperature of a constant-temperature stirrer to be 50-100 ℃, wherein a temperature gradient of 10 ℃ is increased from 50 ℃ to about 100 ℃ every ten minutes;
and F, turning off the stirrer, rapidly putting the magnetic boat into an oxidation muffle furnace by using tweezers, putting the magnetic boat into a 95% N2 and 5% H2 test tube furnace after the oxidation time is 3 hours at 700 ℃, and taking out the magnetic boat after the oxidation time is 4 hours at 1300 ℃ to obtain the special layered nano BAM fluorescent powder.
Preferably, the raw materials are specifically Ba (NO 3) 2 0.0261X (0.99.ltoreq.X.ltoreq.0.9) g, mg (NO 3) 2.6H2O 0.0256g, al (NO 3) 3.9H2O 0.375g, eu (NO 3) 3.6H2O 0.0446 (1-X) g, ethylene glycol 0.5mol, polyacrylic acid 2.4g and citric acid 0.2522g.
Preferably, the concentration of the europium ions is 1%,3%,5%,7% and 10% when the value of X in Ba (NO 3) 2 is 0.99,0.97,0.95,0.93,0.9, respectively, in order to control the content of Eu2+ in the BAM phosphor powder at the optimum concentration of the europium ions. Thus, BAM fluorescent powder with the optimal europium ion concentration is obtained, and when the europium ion concentration is 1 mol%, the nano-size of the BAM is minimum and is about 270nm, and the larger the europium ion concentration is, the larger the BAM size is.
Preferably, after the europium ion concentration is determined, the oxidation temperature needs to be adjusted, the temperature is set at 700 ℃,750 ℃ and 800 ℃, and the BAM fluorescent powder has the optimal size at 700 ℃ and is about 420 nm.
Preferably, when the europium ion concentration is 1%, the oxidation temperature is 700 ℃, the ratio of polyacrylic acid to citric acid is regulated, and three intervals of 2:2,2.5:1.5 and 3:1 are respectively set, the BAM size is found to be optimally between 200nm and 450nm when the europium ion concentration is 2.5:1.5.
Compared with the related art, 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, wherein polyacrylic acid is introduced to generate an electric double layer effect, so that like charges repel each other, and therefore mixed ions in BAM can generate a good dispersing effect, and citric acid can trap each ion and polyacrylic acid to form a 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 original tool beaker used in the reaction is replaced by a magnetic boat, so that the optimal foaming effect can be achieved, and in addition, the oxidation temperature is reduced by 200-300 ℃ compared with the traditional process, so that the reaction time is greatly shortened.
Drawings
FIG. 1 is a flow chart of a bubble method preparation process of a layered nano BAM phosphor provided by the invention.
Detailed Description
The invention will be further described with reference to the drawings and embodiments.
Referring to FIG. 1 in combination, FIG. 1 is a flow chart showing a bubble method preparation process of layered nano BAM fluorescent powder, wherein a cuboid magnetic boat is adopted to replace an original beaker container, then citric acid and polyacrylic acid are introduced, bubbles are formed in the process of constant temperature stirring, the layered nano BAM fluorescent powder is formed by the bubbles at the oxidation temperature, the specific steps are that firstly, the stoichiometric ratio of each element in Ba1-xEuxMgAl10O17 is determined, the stoichiometric ratio of each element in Ba (NO 3) 2 is 0.0261X (0.99 is less than or equal to 0.9) g, mg (NO 3) 2.6H2O is 0.0256g, al (NO 3) 3.9H2O is 0.375g, eu (NO 3) 3.6H2O is 0.0446 (1-X) g, ethylene glycol is 0.5mol, polyacrylic acid is 2.4g, citric acid is 0.2522g, the required raw materials of the BAM matrix are poured into 200ml of A, and 50ml of distilled water is added, stirring with glass rod for 30min, stirring with constant temperature magnetic stirrer at room temperature 150r/min for 30min, pouring citric acid into 100ml beaker B, adding 50ml distilled water, stirring until water is clear, pouring solution in beaker B into beaker A to obtain clear mixed liquid, keeping constant temperature of 50deg.C, stirring for 1 hr/min, pouring polyacrylic acid into beaker A, stirring at original speed until solution is clear, colorless and transparent, adding 0.5mol of ethylene glycol, detecting pH test paper to 9-10, pouring mixed solution of beaker A into cooled and sterilized magnetic boat, regulating temperature of constant temperature stirrer to 50-100deg.C, increasing temperature of 10 deg.C from 50deg.C to 100deg.C every ten minutes, turning off the stirrer, rapidly placing magnetic boat into oxidation muffle with tweezers, and (3) after the oxidation time of 3 hours at 700 ℃, putting the mixture into a 95% N2 and 5% H2 test tube furnace for 4 hours at 1300 ℃ and taking out the mixture to obtain the special layered nano BAM fluorescent powder.
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 chemical formula Ba0.99Eu0.01MgAl10O17, 0.258g of Ba (NO 3) 2 (A.R), 0.256g of Mg (NO 3) 2.6H2O (A.R), 3.75g of Al (NO 3) 3.9H2O (4N) and 0.0045g of Eu (NO 3) 3.6H2O (4N) are accurately weighed, a mixed ion solution is placed in a beaker A containing 200ml of distilled water, stirred for half a hour by a glass rod, placed on a stirrer, then 2.522g of C6H8O7 (A.R) and 24g of polyacrylic acid (A.R) are weighed, placed in a beaker B containing 200ml of distilled water, and stirred to be transparent by the same method. Beaker A and beaker B were mixed and placed in a large beaker, 5 ml of ethylene glycol was added, and after stirring for 10-20min, the mixture was detected to be in the range of 9-10 with pH paper. At this time, the mixed solution was transferred into a magnetic boat, the temperature of a constant temperature magnetic stirrer was controlled, and the speed was accelerated from 50℃to 100℃at a speed of 10℃per hour until the solution began to foam, and the stirrer was rapidly removed. And (3) placing the magnetic boat into an oxidation muffle furnace at 700 ℃ for 3 hours, oxidizing the magnetic boat for 4 hours at 1400 ℃ in a test tube furnace at 5% H2/95% N2, and taking out the magnetic boat to obtain the layered nano BAM fluorescent powder.
Example 2: preparation of Ba0.97Eu0.03MgAl10O17 fluorescent powder
Except that 0.258g of "Ba (NO 3) 2 (A.R) in example 1 was changed to 0.253g of" Ba (NO 3) 2 (A.R), 0.0045g of "Eu (NO 3) 3.6H2O (4N) in example 1 was changed to 0.0135g of" Eu (NO 3) 3.6H2O (4N), and the same conditions as in example 1 were used, ba0.97Eu0.03MgAl10O17 blue phosphor was obtained.
Example 3: preparation of Ba0.95Eu0.05MgAl10O17 fluorescent powder
Except that 0.258g of "Ba (NO 3) 2 (A.R) in example 1 was changed to 0.248g of" Ba (NO 3) 2 (A.R), and 0.0045g of "Eu (NO 3) 3.6H2O (4N) in example 1 was changed to 0.0225g of" Eu (NO 3) 3.6H2O (4N), the same conditions as in example 1 were used to obtain Ba0.97Eu0.03MgAl10O17 blue phosphor.
Example 4: preparation of Ba0.93Eu0.07MgAl10O17 fluorescent powder
Except that 0.258g of "Ba (NO 3) 2 (A.R) in example 1 was changed to 0.243g of" Ba (NO 3) 2 (A.R), 0.0045g of "Eu (NO 3) 3.6H2O (4N) in example 1 was changed to 0.0315g of" Eu (NO 3) 3.6H2O (4N), and the same conditions as in example 1 were used to obtain Ba0.93Eu0.07MgAl10O17 blue phosphor.
Example 5: preparation of Ba0.9Eu0.1MgAl10O17 fluorescent powder
Except that 0.258g of "Ba (NO 3) 2 (A.R) in example 1 was changed to 0.235g of" Ba (NO 3) 2 (A.R), and 0.0045g of "Eu (NO 3) 3.6H2O (4N) in example 1 was changed to 0.045g of" Eu (NO 3) 3.6H2O (4N), the same conditions as in example 1 were used to obtain Ba0.9Eu0.1MgAl10O17 blue phosphor.
Compared with the related art, 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 achieved by introducing the proportion of polyacrylic acid and citric acid, the original tool beaker used for reaction is changed into 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 shortened, and the problem that europium ions are likely to be agglomerated when the BAM fluorescent powder is prepared in the prior art is solved.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (2)
1. A bubble method process for preparing layered nano BAM fluorescent powder is characterized in that a rectangular magnetic boat is adopted to replace an original beaker container, then citric acid and polyacrylic acid are introduced, bubbles are formed in the process of constant temperature stirring, the bubbles form the layered nano BAM fluorescent powder at the oxidation temperature, and the molecular general formula of the layered nano BAM fluorescent powder is Ba 1- x Eu x MgAl 10 O 17 Wherein x is europium ion Eu 2+ Substituted barium ion Ba 2+ X is more than or equal to 0.01 and less than or equal to 0.1, and polyacrylic acid is more than or equal to 1: citric acid is less than or equal to 3, and the preparation steps of the layered nano BAM fluorescent powder are as follows;
step A, firstly determining that Ba 1-x Eu x MgAl 10 O 17 The stoichiometric ratio of each element is 0.0001mol as unit variable, each component raw material is weighed, and the raw material in the step A is specifically Ba (NO 3 ) 2 0.0261Xg, mg (NO 3 ) 2 ·6H 2 O is 0.0256g, al (NO) 3 ) 3 ·9H 2 O is 0.375g, eu (NO 3 ) 3 ·6H 2 O is 0.0446 (1-X) g, ba (NO) 3 ) 2 The values of X in 0.0261X are respectively 0.99,0.97,0.95,0.93 and 0.9, and the concentration variable of europium ions1%,3%,5%,7%, 10%;
pouring raw materials required by the BAM matrix into a 200ml beaker A, adding 50ml distilled water, stirring for 30min by using a glass rod, then placing on a constant-temperature magnetic stirrer, stirring for 30min at the normal temperature of 150r/min, pouring 0.2522g citric acid into a 100ml beaker B, and adding 50ml distilled water, and stirring until the water is clear;
pouring the solution in the beaker B into the beaker A to obtain clear mixed liquid, keeping the temperature at 50 ℃ and stirring for 1h at 300r/min, pouring 2.4g of polyacrylic acid into the beaker A, and continuing stirring at the original speed until the solution is clear, colorless and transparent;
step D, after adding 0.5mol of glycol, detecting the pH test paper to be in a range between 9 and 10,
step E, pouring the mixed solution of the beaker A into a cooled and sterilized magnetic boat, and adjusting the temperature of a constant-temperature stirrer to be 50-100 ℃, wherein a temperature gradient of 10 ℃ is added from 50 ℃ to 100 ℃ every ten minutes;
f, turning off the stirrer, rapidly placing the magnetic boat into an oxidation muffle furnace by using tweezers, oxidizing at 700 ℃ for 3 hours, and then placing 95% N 2 And 5%H 2 And (3) reacting for 4 hours at 1300 ℃ in a test tube furnace, and taking out the layered nano BAM fluorescent powder.
2. The bubble method process of the layered nano BAM fluorescent powder according to claim 1, wherein the europium ion concentration is 1%, the oxidation temperature is 700 ℃, and the ratio of polyacrylic acid to citric acid is regulated to be 2:2,2.5:1.5 or 3:1.
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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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| "钇铝石榴石粉体的低温合成及YAG透明陶瓷的快速制备";李鸣;《中国优秀硕士论文全文数据库 工程科技Ⅰ辑》;20170315(第03期);第B015-841页 * |
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