CN114940901A - Yellow composite fluorescent pigment and preparation method thereof - Google Patents
Yellow composite fluorescent pigment and preparation method thereof Download PDFInfo
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- CN114940901A CN114940901A CN202210781814.8A CN202210781814A CN114940901A CN 114940901 A CN114940901 A CN 114940901A CN 202210781814 A CN202210781814 A CN 202210781814A CN 114940901 A CN114940901 A CN 114940901A
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- 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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- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- C—CHEMISTRY; METALLURGY
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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
- C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
- C09K11/7792—Aluminates
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Abstract
The invention discloses a yellow composite fluorescent pigment and a preparation method thereof. Weighing raw materials according to the stoichiometric ratio of each element in the chemical formula of the blue light excited yellow fluorescent powder, and preparing the blue light excited yellow fluorescent powder by a high-temperature solid-phase method; weighing raw materials according to the stoichiometric ratio of each element in the chemical formula of the near ultraviolet excited blue fluorescent powder, and preparing the near ultraviolet excited blue fluorescent powder by a high-temperature solid phase method; mixing to form mixed fluorescent powder; mixing a main agent and a curing agent to form a film raw material; and adding the mixed fluorescent powder into the film raw material, fully mixing, precuring in an oven, and curing to obtain the yellow composite fluorescent pigment. The composite fluorescent pigment expands the excitable spectrum range of the yellow fluorescent powder and improves the luminous intensity of the yellow fluorescent powder, thereby further expanding the application range of the fluorescent powder in the pigment.
Description
Technical Field
The invention belongs to the technical field of rare earth luminescent materials, relates to a novel yellow composite fluorescent pigment, and also relates to a preparation method of the composite fluorescent pigment.
Background
Fluorescent pigments broadly refer to substances that absorb light of one wavelength and emit light of another wavelength greater than the wavelength of the absorbed light. When ultraviolet light or some light is irradiated on the fluorescent pigment, the fluorescent pigment absorbs energy corresponding to its characteristic frequency, and transits from a ground state to an excited state with higher energy. Atoms in an unstable excited state will transfer and relax to the lowest vibrational level of the excited state, the equilibrium excited state, for a brief period of time, from where they fall back to the higher vibrational level of the ground state. Energy is attenuated in the form of fluorescence during the fall-back process, and the fluorescence disappears immediately when the irradiation is stopped.
Fluorescent pigments are classified into inorganic fluorescent pigments (such as fluorescent pigments used for fluorescent lamps and fluorescent inks for forgery prevention) and organic fluorescent pigments (also called daylight fluorescent pigments): only substances with specific chemical structures will have fluorescent properties. These fluorescent colorants themselves often have inherent deficiencies in light and solvent resistance. One way to overcome these inherent deficiencies is to fuse them chemically or physically into the framework of a polymeric material and further process them into pigments. The polymer material used for the purpose not only plays a role of a solvent of the fluorescent colorant, but also provides protection for the fluorescent colorant, so that the fluorescent colorant is endowed with better performances such as light resistance, solvent resistance and the like.
Blue light excitation of Ce 3+ The doped yttrium aluminum garnet phosphor powder is the earliest and most mature yellow phosphor powder and has the chemical molecular formula of Y 3 A1 5 O 12 :Ce 3+ And can also be abbreviated as YAG: Ce. The most common widely used commercial fluorescent powder YAG can be used as a good fluorescent pigment, and has the advantages that the aluminate fluorescent powder is used as a compound with very stable physical and chemical properties, has excellent luminous performance and good reliability, high brightness and wide emission peak, and meanwhile, the production process of the YAG fluorescent powder is relatively fixed, the synthesis is easy, and the price of raw materials is relatively low. The YAG fluorescent powder has the defects of low color rendering index, narrow excitation wave band and limited application range, and only can absorb part of visible light.
Disclosure of Invention
The invention aims to provide a yellow composite fluorescent pigment which can improve the color rendering index of YAG, widen the absorbable spectral range of YAG and expand the application range of YAG.
The invention also aims to provide a preparation method of the yellow composite fluorescent pigment.
In order to realize the purpose, the technical scheme adopted by the invention is as follows: a yellow composite fluorescent pigment is prepared by mixing blue light excited yellow fluorescent powder, near ultraviolet excited blue fluorescent powder and film raw materials.
The film raw material consists of a main agent and a curing agent according to the mass ratio of 1-20: 1; the main agent adopts silicon rubber Polydimethylsiloxane (PDMS), epoxy resin, polycarbonate or acrylamide; the curing agent adopts ethyl benzene, vinyl triamine or ethylene diamine.
The yellow phosphor is Ce-doped garnet structure phosphor, specifically Y 3 Al 5 O 12 :Ce 3+ (ii) a The blue fluorescent powder is BaMgAl 10 O 17 ∶Eu 2+ 。
The other technical scheme adopted by the invention is as follows: the preparation method of the yellow composite fluorescent pigment specifically comprises the following steps:
1) according to the stoichiometric ratio of each element in the Ce-doped garnet structure fluorescent powder, respectively taking each raw material Y 2 O 3 、Al(NO 3 ) 3 ·9H 2 O and Ce (NO) 3 ) 3 ·6H 2 O, mixing and grinding to obtain first raw material powder, and adding BaF with the mass being 5% of the mass of the first raw material powder 2 And NH in an amount of 0.5% by mass based on the mass of the first raw material powder 4 F, grinding the mixture uniformly by using an agate mortar, placing the mixture in an alumina crucible, sintering the mixture for 1 to 12 hours at the temperature of 800 to 1500 ℃ in an alumina tube furnace under the condition of introducing a reducing atmosphere, cooling the mixture to room temperature along with the furnace, and grinding the sintered product to prepare the Ce-doped garnet-structure fluorescent powder;
according to the chemical formula BaMgAl 10 O 17 ∶Eu 2+ The stoichiometric ratio of each element in the alloy is Ba (NO) 3 ) 2 、Mg(NO 3 ) 2 ·6H 2 O、Al(NO 3 ) 3 ·9H 2 O and Eu 2 O 3 Mixing and grinding to obtain a second raw material powder, and adding BaF with the mass of 5% of the second raw material powder 2 And NH with the mass of 0.5 percent of the mass of the second raw material powder 4 F, uniformly grinding the mixture by using an agate mortar, placing the mixture into an alumina crucible, sintering the mixture for 1 to 12 hours in an alumina tube furnace at the temperature of 800 to 1500 ℃ under the condition of introducing a reducing atmosphere, cooling the mixture to room temperature along with the furnace, and grinding the product to obtain the blue fluorescent powder BaMgAl 10 O 17 ∶Eu 2+ ；
Reducing atmosphere of 95% N by volume 2 And 5% of H 2 And (4) forming.
2) Mixing yellow fluorescent powder and blue fluorescent powder according to the mass ratio of 1: 0.5-2 to form mixed fluorescent powder;
respectively taking the main agent and the curing agent according to the mass ratio of 1-20: 1, and mixing to form a film raw material;
the main agent adopts silicon rubber Polydimethylsiloxane (PDMS), epoxy resin, polycarbonate or acrylamide; the curing agent adopts ethyl benzene, vinyl triamine or ethylene diamine.
3) Taking a film raw material, taking mixed fluorescent powder with the mass being 5-50% of that of the taken film raw material, adding the taken mixed fluorescent powder into the taken film raw material, putting the mixture into a vacuum centrifuge for full mixing, putting the mixture into an oven for pre-curing for 0.5-6 hours at the temperature of 20-180 ℃, and curing for 0.5-10 hours at the temperature of 100-300 ℃ to obtain the yellow composite fluorescent pigment.
The mixed phosphors may also be cured in glass, ceramic, or paint.
The preparation method of the invention mixes the yellow fluorescent powder and the blue fluorescent powder and loads the mixture into a film material to prepare the yellow composite fluorescent pigment. The blue fluorescent powder can absorb ultraviolet light which cannot be absorbed by the yellow fluorescent powder, and meanwhile, the emission peak position of the blue fluorescent powder is superposed with the excitation peak position of the yellow fluorescent powder, so that the luminous intensity and the application range of the yellow fluorescent powder are improved by utilizing the property. However, only mixing two phosphors does not allow efficient light transmission. When light enters the optically denser medium with a large refractive index into the optically thinner medium with a small refractive index, the refraction angle is larger than the incidence angleOptical transmission can be better performed in optically dense media. According to the invention, by utilizing the property that the refractive index of the fluorescent powder in the film material is larger than that in the air, the fluorescence generated after the blue fluorescent powder is excited by ultraviolet light is reflected on the film material interface and transmitted to the yellow fluorescent powder, so that the fluorescence intensity is further improved. Phosphors such as YAG Ce and BaMgAl 10 O 17 Since Eu has a refractive index of 1.55 to 1.60, the refractive index of the host is preferably 1.4 to 1.6, more preferably 1.5 to 1.6. Since the refractive index (total reflection, etc.) of light at the interface between the phosphor and the resin tends to be greatly reduced when the refractive index of the phosphor is close to that of the resin, the light is efficiently transferred from blue to yellow. The yellow fluorescent powder is excited by visible light to emit fluorescence, and the blue fluorescent powder is excited by ultraviolet light to emit fluorescence again to obtain yellow fluorescence. The two powders can also be dispersed in the ceramic or glass, since the refractive index of the ceramic or glass (typically over 1.4) is much higher than that of air, increasing the transmission of light from the blue phosphor to the yellow phosphor, increasing the brightness of the yellow color of the outdoor panel.
The preparation method adopts a high-temperature solid-phase method in the prior art to prepare the yellow fluorescent powder and the blue fluorescent powder, and then the yellow fluorescent powder and the blue fluorescent powder are mixed and prepared in the film material. Compared with the yellow fluorescent powder which can only be excited by visible light to generate fluorescence, the yellow composite fluorescent pigment of the invention superposes the light of the visible light and the blue fluorescent powder, so that the brightness of the yellow fluorescent powder is effectively improved, and the luminous intensity can be improved by more than 10 percent even if the yellow fluorescent powder is commercial powder. The excitable spectrum range of the yellow fluorescent powder is expanded, and the fluorescence intensity of the yellow fluorescent powder is improved, so that the application range of the yellow fluorescent powder is further expanded.
Drawings
FIG. 1 is a comparison graph of emission spectra of a mixed powder and a yellow phosphor obtained by mixing the yellow phosphor and the blue phosphor prepared in example 1 only by mechanical grinding.
FIG. 2 is a graph of data comparing the yellow composite phosphor pigment of example 1 with a YAG commercial phosphor in a spectral color luminometer.
FIG. 3 is an emission spectrum of the yellow composite fluorescent pigment prepared in examples 1 to 3 under excitation of blue light with a wavelength of 380 nm.
FIG. 4 is a picture of a yellow composite fluorescent pigment prepared in examples 1-3 under visible light.
FIG. 5 is a photograph of the yellow composite fluorescent pigment prepared in examples 1 to 3 under an ultraviolet lamp.
Detailed Description
The following description of the embodiments of the present invention will be further described with reference to the drawings and examples, but should not be construed as limiting the scope of the invention.
Example 1
According to the formula Y 3 A1 5 O 12 :Ce 3+ The stoichiometric ratio of each element in the formula (I) is Y 2 O 3 、Al(NO 3 ) 3 ·9H 2 O and Ce (NO) 3 ) 3 ·6H 2 O, mixing and grinding to obtain first raw material powder, and adding BaF with the mass being 5% of the mass of the first raw material powder 2 And NH with the mass being 0.5% of the mass of the first raw material powder 4 F, placing the mixture in an alumina crucible, introducing 95 percent by volume of N into an alumina tube furnace 2 And 5% of H 2 Sintering the mixture at 1500 ℃ for 5h in a reducing atmosphere, cooling the mixture to room temperature along with the furnace, and grinding the calcined product to obtain the yellow fluorescent powder Y 3 A1 5 O 12 :Ce 3+ (ii) a According to the chemical formula BaMgAl 10 O 17 ∶Eu 2＋ The stoichiometric ratio of each element in the alloy is Ba (NO) 3 ) 2 、Mg(NO 3 ) 2 ·6H 2 O、Al(NO 3 ) 3 ·9H 2 O and Eu 2 O 3 Mixing, grinding, mixing and grinding to obtain a second raw material powder, and adding BaF with the mass of 5% of the second raw material powder 2 And NH with the mass of 0.5 percent of the mass of the second raw material powder 4 F, placing the mixture in an alumina crucible, introducing 95 percent by volume of N into an alumina tube furnace 2 And 5% of H 2 Sintering the mixture for 5 hours at 1500 ℃, cooling the mixture to room temperature along with the furnace, grinding the product to obtain the blue fluorescent powder BaMgAl 10 O 17 ∶Eu 2＋ (ii) a Weighing 1.89Mixing silicone rubber, polydimethylsiloxane and 0.21g of ethylbenzene to form a film raw material; taking 0.2g of yellow fluorescent powder and 0.1g of blue fluorescent powder, mixing, adding the mixture into a film raw material, putting the film raw material into a vacuum centrifuge for full mixing, placing the film raw material into an oven for precuring for 0.5 hour at the temperature of 60 ℃, and curing for 2 hours at the temperature of 100 ℃; the yellow composite fluorescent pigment is prepared.
FIG. 1 is a comparison graph of emission spectra of a mixed powder and a yellow phosphor obtained by mixing a yellow phosphor and a blue phosphor prepared in example 1 only by mechanical grinding. It can be seen from fig. 1 that the emission intensity of the yellow phosphor is not improved by mechanically grinding and mixing the yellow and blue phosphors.
FIG. 2 is a graph of comparative data between the yellow composite fluorescent pigment prepared in example 1 and a YAG commercial phosphor in a spectral color illuminometer. FIG. 2 shows that the fluorescence intensity is obviously improved by not less than 10% after the blue fluorescent powder is added into the yellow fluorescent powder and the film raw material is added.
Example 2
According to formula (Y) 2.5 Ce 0.5 )Al 5 O 12 The stoichiometric ratio of each element in the formula (I) is Y 2 O 3 、Al(NO 3 ) 3 ·9H 2 O and Ce (NO) 3 ) 3 ·6H 2 O, mixing and grinding to obtain first raw material powder, and adding BaF accounting for 5% of the mass of the first raw material powder 2 And NH in an amount of 0.5% by mass based on the mass of the first raw material powder 4 F, grinding the mixture evenly by using an agate mortar, placing the mixture in an alumina crucible, and introducing 95 percent by volume of N into an alumina tube furnace at the temperature of 800 DEG C 2 And 5% of H 2 Sintering for 1h under the condition of reducing atmosphere, cooling to room temperature along with the furnace, grinding the sintered substance to obtain the yellow fluorescent powder (Y) 2.5 Ce 0.5 )Al 5 O 12 . Mixing the reactants according to a stoichiometric proportion, grinding, and then placing in a high-temperature furnace for sintering. Calcining at 1000 deg.C in air for 24 hr, mixing, and sintering at 1500 deg.C in air for 24 hr to obtain the desired Y 3 A1 5 O 12 :Ce 3+ And (3) yellow fluorescent powder. According to the chemical formula BaMgAl 10 O 17 ∶Eu 2+ Taking Ba (NO) as the stoichiometric ratio of each element 3 ) 2 、Mg(NO 3 ) 2 ·6H 2 O、Al(NO 3 ) 3 ·9H 2 O and Eu 2 O 3 (99.99%), mixing and grinding to obtain a second raw material powder, and adding BaF with the mass of 5% of the second raw material powder 2 And NH with the mass of 0.5 percent of the mass of the second raw material powder 4 F, uniformly grinding the mixture by using an agate mortar, placing the mixture in an alumina crucible, heating the mixture in an alumina tube furnace at 1100 ℃ and introducing 95 percent by volume of N 2 And 5% of H 2 Sintering for 12h under the condition of reducing atmosphere, cooling to room temperature along with the furnace, grinding the product to obtain the blue fluorescent powder BaMgAl 10 O 17 ∶Eu 2+ (ii) a Mixing yellow fluorescent powder and blue fluorescent powder respectively according to the mass ratio of 1: 1 to form mixed fluorescent powder; respectively mixing epoxy resin and vinyl triamine at a mass ratio of 20: 1 to form a film raw material; taking a film raw material, taking mixed fluorescent powder with the mass being 50% of the mass of the taken film raw material, adding the taken mixed fluorescent powder into the taken film raw material, putting the mixture into a vacuum centrifuge for full mixing, putting the mixture into an oven for precuring for 6 hours at the temperature of 20 ℃, and curing for 6 hours at the temperature of 200 ℃ to obtain the yellow composite fluorescent pigment.
Example 3
According to formula (Y) 2.5 Ce 0.5 )Al 5 O 12 The stoichiometric ratio of each element in (A), (B) and (C) is taken 2 O 3 、Al(NO 3 ) 3 ·9H 2 O and Ce (NO) 3 ) 3 ·6H 2 O, mixing and grinding to obtain first raw material powder, and adding BaF accounting for 5% of the mass of the first raw material powder 2 And NH in an amount of 0.5% by mass based on the mass of the first raw material powder 4 F, grinding the mixture evenly by using an agate mortar, placing the mixture in an alumina crucible, and introducing 95 percent N by volume into an alumina tubular furnace at 1200 DEG C 2 And 5% of H 2 Sintering for 12h under the condition of reducing atmosphere, cooling to room temperature along with the furnace, grinding the sintered product to obtain the yellow fluorescent powder (Y) 2.5 Ce 0.5 )Al 5 O 12 . Chemical formula BaMgAl 10 O 17 ∶Eu 2+ The stoichiometric ratio of each element in the alloy is Ba (NO) 3 ) 2 、Mg(NO 3 ) 2 ·6H 2 O、Al(NO 3 ) 3 ·9H 2 O and Eu 2 O 3 Mixing and grinding to obtain a second raw material powder, and adding BaF with the mass of 5% of the second raw material powder 2 And NH with the mass of 0.5 percent of the mass of the second raw material powder 4 F, uniformly grinding the mixture by using an agate mortar, placing the mixture in an alumina crucible, sintering the mixture for 1 hour in an alumina tube furnace at the temperature of 800 ℃ under the condition of introducing a reducing atmosphere, cooling the mixture to room temperature along with the furnace, and grinding the product to obtain the blue fluorescent powder BaMgAl 10 O 17 ∶Eu 2+ (ii) a Mixing yellow fluorescent powder and blue fluorescent powder respectively according to the mass ratio of 1: 2 to form mixed fluorescent powder; respectively taking polycarbonate and ethylenediamine according to the mass ratio of 1: 1, and mixing to form a film raw material; taking a film raw material, taking mixed fluorescent powder with the mass being 5% of the mass of the taken film raw material, adding the taken mixed fluorescent powder into the taken film raw material, putting the mixture into a vacuum centrifuge for full mixing, putting the mixture into an oven for precuring for 3 hours at the temperature of 180 ℃, and curing for 10 hours at the temperature of 300 ℃ to obtain the yellow composite fluorescent pigment.
FIG. 3 is an emission spectrum of the yellow composite fluorescent pigment prepared in examples 1 to 3 under excitation of blue light with a wavelength of 380 nm. It can be seen that as the addition amount of the blue phosphor increases, the enhanced yellow fluorescence tends to increase first and then decrease, so that a better doping ratio can be obtained for later application.
FIG. 4 is a picture of a yellow composite fluorescent pigment prepared in examples 1-3 under visible light. FIG. 5 is a photograph of the yellow composite fluorescent pigment prepared in examples 1-3 under an ultraviolet lamp. From fig. 4 and fig. 5, it can be found that the yellow color of the yellow composite fluorescent sample added with the blue fluorescent powder is obviously stronger than that of the pure yellow fluorescent powder under visible light.
Claims (5)
1. The yellow composite fluorescent pigment is characterized by being prepared by mixing yellow fluorescent powder excited by blue light, blue fluorescent powder excited by near ultraviolet and a thin film material.
2. The yellow composite fluorescent pigment of claim 1, wherein the yellow phosphor is Ce-doped garnet structure phosphor, and the blue phosphor is BaMgAl 10 O 17 Eu, the film material is formed by mixing a main agent and a curing agent, wherein the main agent adopts silicone rubber polydimethylsiloxane, epoxy resin, polycarbonate or acrylamide; the curing agent adopts ethyl benzene, vinyl triamine or ethylene diamine.
3. The preparation method of the yellow composite fluorescent pigment of claim 1 is characterized by comprising the following steps:
1) according to the stoichiometric ratio of each element in the chemical formula of the yellow fluorescent powder excited by blue light, respectively taking each raw material, mixing and grinding the raw materials to obtain first raw material powder, adding BaF with the mass of 5 percent of the mass of the first raw material powder 2 And NH in an amount of 0.5% by mass based on the mass of the first raw material powder 4 F, uniformly grinding the mixture by using an agate mortar, placing the mixture into an alumina crucible, and sintering the mixture for 1 to 12 hours in an alumina tube furnace at the temperature of 800 to 1500 ℃ under the condition of introducing a reducing atmosphere to prepare yellow fluorescent powder excited by blue light;
according to the stoichiometric ratio of each element in the chemical formula of the near ultraviolet excited blue fluorescent powder, respectively taking the raw materials, mixing and grinding the raw materials to obtain second raw material powder, and adding BaF with the mass of 5 percent of the mass of the second raw material powder 2 And NH with the mass of 0.5 percent of the mass of the second raw material powder 4 F, uniformly grinding the mixture by using an agate mortar, placing the mixture into an alumina crucible, sintering the mixture for 1 to 12 hours at the temperature of 800 to 1500 ℃ in an alumina tube furnace under the condition of introducing a reducing atmosphere, cooling the mixture to room temperature along with the furnace, and grinding the mixture to obtain near-ultraviolet excited blue fluorescent powder;
2) mixing yellow fluorescent powder excited by blue light and blue fluorescent powder excited by near ultraviolet respectively according to the mass ratio of 1: 0.5-2 to form mixed fluorescent powder;
respectively taking the main agent and the curing agent according to the mass ratio of 1-20: 1, and mixing to form a film raw material;
3) taking a film raw material, taking mixed fluorescent powder with the mass being 5-50% of the mass of the taken film raw material, adding the taken mixed fluorescent powder into the taken film raw material, fully mixing in a vacuum centrifuge, precuring for 0.5-6 hours in an oven at the temperature of 20-180 ℃, and curing for 0.5-10 hours at the temperature of 100-300 ℃ to obtain the yellow composite fluorescent pigment.
4. The method for preparing the yellow composite fluorescent pigment of claim 3, wherein the main agent is silicone rubber polydimethylsiloxane, epoxy resin, polycarbonate or acrylamide.
5. The method of claim 3, wherein the curing agent is ethylbenzene, vinyltriamine or ethylenediamine.
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