CN111187532A - BAM-based automobile paint with fluorescent whitening effect and preparation method thereof - Google Patents
BAM-based automobile paint with fluorescent whitening effect and preparation method thereof Download PDFInfo
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/22—Luminous paints
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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
- C09K11/7734—Aluminates
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Abstract
A fluorescent whitening automobile paint based on BAM and a preparation method thereof are disclosed, which comprises an optical functional material and a carrier material, wherein the optical functional material is magnesium barium aluminate-based blue fluorescent powder with nanoscale, and the carrier material is automobile varnish; after the two are compounded according to the mass compounding ratio of 10-50%, the two are coated on the surface of the white primer of the automobile. The chemical general formula of the optical functional material is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ion Eu2+ to barium ion Ba2+, and x is more than or equal to 0.40 and less than or equal to 0.80. The invention consists of NH4Chemical initiation of Cl, grain boundary separation of nano particles and ultrahigh europium ion Eu2+The concentration exchange coupling of the three components is acted together to lead the europium ion Eu in the obtained nanometer BAM fluorescent powder2+The ultralimit energy level fission occurs, so that the BAM fluorescent powder can effectively absorb the near ultraviolet radiation of the sun, and can be seamlessly dissolved into the automobile varnish due to the nanoscale of the particles to obtain the fluorescent whitening automobile paint. The paint is used in sunshineThe ultra-strong blue fluorescence is emitted, and the fluorescent whitening effect can be obviously embodied by matching with white primer of an automobile.
Description
Technical Field
The invention relates to a BAM-based automobile fluorescent whitening paint and a preparation method thereof, belonging to the technical field of automobile paint.
Background
Blue light has a significant whitening effect on white, while BAM (Ba)1-xEuxMgAl10O17) The fluorescent powder can emit blue fluorescent light under the excitation of ultraviolet light or near ultraviolet light, and sunlight contains abundant ultraviolet light and near ultraviolet light. Therefore, the BAM fluorescent powder can be dissolved in the automotive varnish to obtain the automotive composite paint, and the white automobile can show an obvious fluorescent whitening effect under the excitation of sunlight by matching with the white primer of the automobile, so that a very beautiful white automobile is constructed.
In the near ultraviolet light of the sun, the number of photons at 380nm is far greater than that at 335nm, so far, the conventional BAM fluorescent powder cannot fully utilize the solar radiation at 380nm, and the ratio of the excitation intensity at 380nm to that at 335nm is only 25-60% (Zhou, Y.; Lin, J).Journal of Solid State Chemistry2005,178(2), 441-447；Lu, C.-H.; Chen, C.-T.; Bhattacharjee, B.Journal of Rare Earths2006,24(6), 706-711；Zhang, W.; He, D.; Ma, G.; Cui, S.; Li, G.;Jiao, H.Journal of Physics and Chemistry of Solids2014,75(2), 163-167). Therefore, conventional BAM phosphors cannot be applied to fluorescent whitening automotive paints.
Disclosure of Invention
The invention aims to provide a BAM-based automobile fluorescent whitening paint, and aims to provide a preparation method of a light functional material in the automobile fluorescent whitening paint, which shows ultra-strong blue fluorescence under near ultraviolet excitation and can be dissolved in automobile varnish without trace.
The technical scheme adopted by the invention is as follows:
the fluorescent whitening automobile paint based on the BAM is composed of an optical functional material and a carrier material, wherein the optical functional material is magnesium barium aluminate-based blue fluorescent powder with a nanoscale, and the carrier material is automobile varnish; the mass compounding ratio of the optical functional material to the carrier material is 10-50%, and after compounding, the optical functional material is coated on the surface of the white primer of the automobile, so that the fluorescent whitening effect can be shown under the irradiation of outdoor sunlight.
The chemical general formula of the optical functional material is Ba1-xEuxMgAl10O17, wherein x is the molar ratio of europium ion Eu2+ to barium ion Ba2+, and x is more than or equal to 0.40 and less than or equal to 0.80.
The preparation method of the optical functional material comprises the following steps: firstly, accurately weighing Ba (NO3)2, Mg (NO3) 2.6H 2O, Al (NO3) 3.9H 2O and Eu (NO3) 3.6H 2O according to the stoichiometric ratio of each element in a chemical formula of Ba1-xEuxMgAl10O17, and dissolving the Ba (NO3)2, the Mg (NO3) 2.6H 2O, the Eu (NO3) 3.6H 2O in deionized water to obtain a first solution, wherein the molar ratio of Eu (NO3) 3.6H 2O is more than or equal to 0.40 and less than or equal to 0.80; secondly, dissolving required amount of (NH4)2CO3 in deionized water to obtain a second solution; step three, dropwise adding the first solution into the second solution, uniformly mixing and stirring, and then adding an ammonia water solution to adjust the pH of a precipitation system to obtain a precipitate; fourthly, after the precipitation reaction is finished, performing centrifugal separation, pouring out supernatant liquor, and drying the precipitate in a drying oven at the temperature of 120 ℃ for 6-8 hours to obtain white precursor fluffy powder; fifthly, adding 0.5wt% of NH4Cl serving as a chemical initiator into the white precursor, transferring the mixed powder into a corundum crucible, putting the corundum crucible into a tubular furnace with 95% of N2 and 5% of H2 in a reducing atmosphere, heating to 1350 ℃, calcining for 8 hours, cooling the furnace, taking out the fired product, and grinding again to obtain the nano BAM fluorescent powder with the particle size smaller than 500 nm.
In the third step, the first solution is dropwise added into the second solution, and the mixing and stirring speed is 350r/min to 400 r/min.
In the fifth step, the white precursor powder is heated at a rate of 5 to 10 ℃/min in a reducing atmosphere of 95% N2 and 5% H2.
Nano BAM (Ba) prepared by the invention1-xEuxMgAl10O17X is more than or equal to 0.40 and less than or equal to 0.80) fluorescent powder due to NH4Chemical initiation of Cl, grain boundary separation of nano particles and ultrahigh europium ion Eu2+The concentration exchange coupling of the three components can act together to ensure that europium ion Eu in the nano BAM fluorescent powder2+The over-limit energy level fission is generated, thereby leading the Eu as the luminescence center2+The excitation spectrum of the solar energy collector is remarkably widened, and the excitation intensity at 380nm is strong, so that the near ultraviolet radiation energy in the sun can be more fully utilized. Meanwhile, the BAM fluorescent material is in a nanometer scale (less than 500 nm), so that the BAM fluorescent material can be dissolved into the automobile varnish without trace. The obtained automobile fluorescent whitening paint can emit strong blue fluorescent light under the irradiation of sunlight, and can embody remarkable fluorescent whitening effect by matching with the white primer of an automobile, thereby constructing a very beautiful white automobile.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of a series of phosphor samples made according to examples 1-5 of the present invention.
FIG. 2 shows Ba prepared according to example 1 of the present invention0.6Eu0.4MgAl10O17SEM image of phosphor sample.
FIG. 3 shows Ba prepared according to example 1 of the present invention0.6Eu0.4MgAl10O17Excitation spectrum of the phosphor sample.
FIG. 4 shows Ba prepared according to example 1 of the present invention0.6Eu0.4MgAl10O17Emission spectrum of the phosphor sample.
FIG. 5 shows Ba prepared according to example 2 of the present invention0.5Eu0.5MgAl10O17Excitation spectrum of the phosphor sample.
FIG. 6 is a drawing showing a view of a structure of an embodiment 2 of the present inventionPrepared Ba0.5Eu0.5MgAl10O17Emission spectrum of the phosphor sample.
FIG. 7 shows Ba prepared in example 3 of the present invention0.4Eu0.6MgAl10O17Excitation spectrum of the phosphor sample.
FIG. 8 shows Ba prepared in example 3 of the present invention0.4Eu0.6MgAl10O17Emission spectrum of the phosphor sample.
FIG. 9 shows Ba prepared according to example 4 of the present invention0.3Eu0.7MgAl10O17Excitation spectrum of the phosphor sample.
FIG. 10 shows Ba prepared according to example 4 of the present invention0.3Eu0.7MgAl10O17Emission spectrum of the phosphor sample.
FIG. 11 shows Ba prepared in example 5 of the present invention0.2Eu0.8MgAl10O17Excitation spectrum of the phosphor sample.
FIG. 12 shows Ba prepared in example 5 of the present invention0.2Eu0.8MgAl10O17Emission spectrum of the phosphor sample.
FIG. 13 shows Ba prepared according to example 1 of the present invention0.6Eu0.4MgAl10O17Comparison of excitation spectra of phosphor samples and BAM commercial powder.
FIG. 14 shows Ba prepared according to example 2 of the present invention0.5Eu0.5MgAl10O17Comparison of excitation spectra of phosphor samples and BAM commercial powder.
FIG. 15 shows Ba prepared according to example 3 of the present invention0.4Eu0.6MgAl10O17Comparison of excitation spectra of phosphor samples and BAM commercial powder.
FIG. 16 shows Ba prepared according to example 4 of the present invention0.3Eu0.7MgAl10O17Comparison of excitation spectra of phosphor samples and BAM commercial powder.
FIG. 17 shows Ba prepared in example 5 of the present invention0.2Eu0.8MgAl10O17Comparison of excitation spectra of phosphor samples and BAM commercial powder.
Detailed Description
The invention is further illustrated by the following specific examples.
The fluorescent whitening automobile paint based on the BAM is composed of an optical functional material and a carrier material, wherein the optical functional material is magnesium barium aluminate-based blue fluorescent powder with a nanoscale, and the carrier material is automobile varnish; the mass compounding ratio of the optical functional material to the carrier material is 10-50%, and after compounding, the optical functional material is coated on the surface of the white primer of the automobile, so that the optical functional material can show an obvious fluorescent whitening effect under the irradiation of outdoor sunlight.
The chemical general formula of the optical functional material is Ba1-xEuxMgAl10O17Wherein x is europium ion Eu2+Substituted barium ion Ba2+X is more than or equal to 0.40 and less than or equal to 0.80.
The preparation method of the optical functional material comprises the following steps: in the first step, according to the formula Ba1-xEuxMgAl10O17The stoichiometric ratio of each element in the Ba (NO) is accurately weighed3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O、Eu(NO3)3·6H2O and dissolving in deionized water to obtain a first solution, wherein Eu (NO)3)3·6H2The molar ratio of O is more than or equal to 0.40 and less than or equal to 0.80; in the second step, the required amount of (NH)4)2CO3Dissolving in deionized water to obtain a second solution; step three, dropwise adding the first solution into the second solution, uniformly mixing and stirring, and then adding an ammonia water solution to adjust the pH of a precipitation system to obtain a precipitate; fourthly, after the precipitation reaction is finished, performing centrifugal separation, pouring out supernatant liquor, and drying the precipitate in a drying oven at the temperature of 120 ℃ for 6-8 hours to obtain white precursor fluffy powder; fifthly, adding NH with the mass fraction of 0.5wt percent as a chemical initiator into the white precursor4Cl, and the mixed powder was subsequently transferred to a corundum crucibleIn, then put into N2Is 95% and H2And (3) heating to 1350 ℃ in a 5% reducing atmosphere tube furnace, calcining for 8h, cooling the furnace, taking out the calcined product, and grinding again to obtain the nano BAM fluorescent powder with the particle size of less than 500 nm. The specific preparation of the optically functional material is illustrated by the following specific examples. According to the method, the raw materials are fully mixed at a molecular level, and the growth of crystal nuclei is limited by controlling reaction conditions, so that the nano-scale BAM fluorescent powder can be obtained. At the same time, NH is added in the method4Cl as chemical initiation and doped with ultra-high concentration of europium ion Eu2+The two conditions and the grain boundary barrier effect of the nano particles act together to ensure that the europium ion Eu at the luminescence center2+The ultralimit energy level fission occurs, so that the BAM fluorescent powder can effectively absorb the solar near ultraviolet radiation with 380nm as the main part.
In the third step, the first solution is dropwise added into the second solution, and the mixing and stirring speed is 350r/min to 400 r/min. If the stirring rate is lower than the parameter range, the crystallization time is increased, so that large particles are formed, and the dissolution into the automobile varnish is not facilitated; if the stirring speed is higher than the parameter range, the particle size is too small, agglomeration is easy to occur, and the growth of crystal grains is influenced.
In the fifth step, the white precursor powder is in N2Is 95% and H2In 5% reducing atmosphere, the heating rate is 5-10 deg.C/min. The temperature rise rate is slow, the appearance is easy to maintain, the crystallinity can be improved, and the required nano fluorescent material can be obtained.
Example 1: ba0.6Eu0.4MgAl10O17Preparation of phosphor
According to the chemical formula Ba0.6Eu0.4MgAl10O17The stoichiometric ratio of each element in the Ba (NO) is accurately weighed3)2(A.R)0.3136 g, Mg (NO)3)2·6H2O (A.R)0.5128 g, Al (NO)3)3·9H2O (4N)7.5026 g, Eu (NO)3)3·6H20.3568 g of O (4N) and dissolved in deionized water to obtain a metal ion mixed solution. Weigh 17 g (NH)4)2CO3Dissolved in 100mL of deionized water to give a 2.16mol/L solution of ammonium carbonate. And (3) adjusting the temperature of the magnetic stirrer to about 30 ℃ at the rotating speed of 350r/min-400r/min, and respectively heating and stirring the metal ion mixed solution and the ammonium carbonate solution until the solid particles are dissolved. Subsequently, the mixed solution of metal ions was slowly dropped thereinto while stirring the ammonium carbonate solution, and after completion of the dropping, 50mL of aqueous ammonia was added to control the pH of the precipitation system to about 9. And after the precipitation reaction is finished, performing centrifugal separation, pouring out supernatant liquor, and drying the precipitate in a drying oven at the temperature of 120 ℃ for 6-8 hours to obtain white precursor fluffy powder. Adding NH with the mass fraction of 0.5wt% into the white precursor4Cl, the mixed powder was subsequently transferred into a corundum crucible and placed in N2Is 95% and H2Heating to 1350 ℃ at the heating rate of 5-10 ℃/min in a tubular furnace with 5% reducing atmosphere, calcining for 8h, cooling the furnace, taking out the fired product, and grinding again to obtain Ba0.6Eu0.4MgAl10O17And blue fluorescent powder.
Example 2: ba0.5Eu0.5MgAl10O17Preparation of phosphor
"Ba (NO) in example 13)2(A.R)0.3136 g "Change to" Ba (NO)3)2(A.R)0.2613 g ", mixing" Eu (NO) in example 13)3·6H2O (4N) 0.3568 g is replaced by Eu (NO)3)3·6H2O (4N) 0.4460 g ", prepared under otherwise the same conditions as in example 1, to give Ba0.5Eu0.5MgAl10O17And blue fluorescent powder.
Example 3: ba0.4Eu0.6MgAl10O17Preparation of phosphor
"Ba (NO) in example 13)2(A.R)0.3136 g "Change to" Ba (NO)3)2(A.R)0.2091 g ", mixing" Eu (NO) in example 13)3·6H2O (4N) 0.3568 g is replaced by Eu (NO)3)3·6H2O (4N) 0.5352 g', other strips preparedBa was obtained in the same manner as in example 10.4Eu0.6MgAl10O17And blue fluorescent powder.
Example 4: ba0.3Eu0.7MgAl10O17Preparation of phosphor
"Ba (NO) in example 13)2(A.R)0.3136 g "Change to" Ba (NO)3)2(A.R)0.1568 g ", mixing" Eu (NO) in example 13)3·6H2O (4N) 0.3568 g is replaced by Eu (NO)3)3·6H2O (4N) 0.6244 g ", prepared under otherwise the same conditions as in example 1, to give Ba0.3Eu0.7MgAl10O17And blue fluorescent powder.
Example 5: ba0.2Eu0.8MgAl10O17Preparation of phosphor
"Ba (NO) in example 13)2(A.R)0.3136 g "Change to" Ba (NO)3)2(A.R)0.1045 g ", mixing" Eu (NO) in example 13)3·6H2O (4N) 0.3568 g is replaced by Eu (NO)3)3·6H2O (4N) 0.7136 g ", prepared under otherwise the same conditions as in example 1, to give Ba0.2Eu0.8MgAl10O17And blue fluorescent powder.
Claims (5)
1. A BAM-based automotive paint with fluorescent whitening characterized by: the fluorescent whitening automobile paint consists of an optical functional material and a carrier material, wherein the optical functional material is magnesium barium aluminate-based blue fluorescent powder with a nanoscale, and the carrier material is automobile varnish; the mass compounding ratio of the optical functional material to the carrier material is 10-50%, and after compounding, the optical functional material is coated on the surface of the white primer of the automobile, so that the fluorescent whitening effect can be shown under the irradiation of outdoor sunlight.
2. A BAM based automotive paint with fluorescent whitening according to claim 1, wherein: the chemical general formula of the optical functional material is Ba1-xEuxMgAl10O17Wherein x is europium ion Eu2+Substituted barium ion Ba2+X is more than or equal to 0.40 and less than or equal to 0.80.
3. A BAM based automotive paint with fluorescence whitening according to claim 2, wherein: the preparation method of the optical functional material comprises the following steps: in the first step, according to the formula Ba1-xEuxMgAl10O17The stoichiometric ratio of each element in the Ba (NO) is accurately weighed3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O、Eu(NO3)3·6H2O and dissolving in deionized water to obtain a first solution, wherein Eu (NO)3)3·6H2The molar ratio of O is more than or equal to 0.40 and less than or equal to 0.80; in the second step, the required amount of (NH)4)2CO3Dissolving in deionized water to obtain a second solution; step three, dropwise adding the first solution into the second solution, uniformly mixing and stirring, and then adding an ammonia water solution to adjust the pH of a precipitation system to obtain a precipitate; fourthly, after the precipitation reaction is finished, performing centrifugal separation, pouring out supernatant liquor, and drying the precipitate in a drying oven at the temperature of 120 ℃ for 6-8 hours to obtain white precursor fluffy powder; fifthly, adding NH with the mass fraction of 0.5wt percent as a chemical initiator into the white precursor4Cl, the mixed powder was subsequently transferred into a corundum crucible and placed in N2Is 95% and H2And (3) heating to 1350 ℃ in a 5% reducing atmosphere tube furnace, calcining for 8h, cooling the furnace, taking out the calcined product, and grinding again to obtain the nano BAM fluorescent powder with the particle size of less than 500 nm.
4. A BAM based automotive paint with fluorescence whitening according to claim 3, wherein: in the third step, the first solution is dropwise added into the second solution, and the mixing and stirring speed is 350r/min to 400 r/min.
5. A BAM-based paint for the fluorescent whitening of automobiles as claimed in claim 3Characterized in that: in the fifth step, the white precursor powder is in N2Is 95% and H2In 5% reducing atmosphere, the heating rate is 5-10 deg.C/min.
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Cited By (3)
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| CN111876152A (en) * | 2020-08-27 | 2020-11-03 | 兰州大学 | Green fluorescent powder for high-quality Micro-LED device and preparation thereof |
| CN111925683A (en) * | 2020-08-27 | 2020-11-13 | 兰州大学 | BAM EM-based fluorescent whitening automobile paint and preparation method thereof |
| CN115074128A (en) * | 2021-03-11 | 2022-09-20 | 兰州大学 | Bubble method preparation process of layered nano BAM fluorescent powder |
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| CN115074128A (en) * | 2021-03-11 | 2022-09-20 | 兰州大学 | Bubble method preparation process of layered nano BAM fluorescent powder |
| CN115074128B (en) * | 2021-03-11 | 2023-11-14 | 兰州大学 | Bubble method preparation process of layered nano BAM fluorescent powder |
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Application publication date: 20200522 |