CN118995204A - Yellow fluorescent material, preparation method and application thereof, high-color-rendering inorganic yellow fluorescent pigment and preparation thereof - Google Patents
Yellow fluorescent material, preparation method and application thereof, high-color-rendering inorganic yellow fluorescent pigment and preparation thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 48
- 239000000049 pigment Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000009877 rendering Methods 0.000 title claims abstract description 20
- 229910052909 inorganic silicate Inorganic materials 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims description 35
- 239000002994 raw material Substances 0.000 claims description 34
- 239000001052 yellow pigment Substances 0.000 claims description 30
- 238000000227 grinding Methods 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 150000001553 barium compounds Chemical class 0.000 claims description 7
- 150000001785 cerium compounds Chemical class 0.000 claims description 7
- 150000002178 europium compounds Chemical class 0.000 claims description 7
- 150000003377 silicon compounds Chemical class 0.000 claims description 7
- 150000003438 strontium compounds Chemical class 0.000 claims description 7
- 238000011161 development Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910002915 BiVO4 Inorganic materials 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 230000005284 excitation Effects 0.000 abstract description 24
- 239000001023 inorganic pigment Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 35
- 230000000052 comparative effect Effects 0.000 description 16
- 238000000295 emission spectrum Methods 0.000 description 14
- 238000000695 excitation spectrum Methods 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- 229910000018 strontium carbonate Inorganic materials 0.000 description 3
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910052693 Europium Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000012860 organic pigment Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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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
- C09K11/7783—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
- C09K11/77922—Silicates
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0006—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black containing bismuth and vanadium
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/34—Compounds of chromium
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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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
- C09K11/02—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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Abstract
The invention provides a yellow fluorescent material, a preparation method and application thereof, and an inorganic yellow fluorescent pigment with high color rendering property and a preparation thereof, belonging to the technical field of luminescent materials. The chemical composition of the yellow fluorescent material provided by the invention is Sr 2‑x‑y‑zBaxSiO4:yCe3+,zEu2+, wherein, x is more than or equal to 0.2 and less than or equal to 1, y is more than or equal to 0.01 and less than or equal to 0.08, and z is more than or equal to 0.1. The yellow fluorescent material has a very wide excitation band, can be effectively excited by near ultraviolet light and blue light, has very strong absorption in a wave band of 300-450 nm, emits yellow light with a main peak of about 550nm, and has higher emission intensity. The inorganic yellow fluorescent pigment prepared by the yellow fluorescent material has obviously enhanced diffuse reflection effect on yellow under sunlight, and effectively improves the color rendering property of the inorganic pigment.
Description
Technical Field
The invention relates to the technical field of luminescent materials, in particular to a yellow fluorescent material, a preparation method and application thereof, and an inorganic yellow fluorescent pigment with high color rendering property and preparation thereof.
Background
In recent years, new yellow phosphors have been reported, wherein the widely studied substrates are free of nitrogen oxides, silicates and aluminates, and have attracted increasing attention. Among them, silicate-based phosphors have many attractive advantages, such as Sr 2SiO4:Eu2+ being capable of emitting bright orange light, excitation spectrum covering the near ultraviolet (380-410 nm) and blue (450-480 nm) ranges, and emission band centered around 562nm, while exhibiting good thermal stability. The luminescent property of the yellow silicate phosphor Sr 2SiO4:Eu2+ is the key for improving the color rendering property of inorganic yellow pigment.
The yellow pigment is a very striking pigment class, and is widely used in the aspects of road signs, indication boards and the like, and the traditional inorganic yellow pigment comprises iron yellow, cadmium chrome yellow, titanium yellow, bismuth yellow and the like. Wherein color is one of the important indicators for measuring the performance of inorganic pigments, so improving the color performance of inorganic yellow pigments is the aim of researchers. However, it is difficult to realize industrialization of the novel yellow pigment developed in recent years. While mixing with an organic pigment helps to improve the color properties of the yellow pigment, disadvantages of the organic pigment such as poor heat and light resistance and weather resistance also indirectly affect the application of the inorganic yellow pigment.
Disclosure of Invention
The invention aims to provide a yellow fluorescent material, a preparation method and application thereof, and an inorganic yellow fluorescent pigment with high color rendering property and a preparation thereof, wherein the yellow fluorescent material can obviously improve the color rendering property of the inorganic yellow pigment.
In order to achieve the above object, the present invention provides the following technical solutions:
The invention provides a yellow fluorescent material, the chemical composition is Sr 2-x-y-zBaxSiO4:yCe3+,zEu2+, wherein, x is more than or equal to 0.2 and less than or equal to 1, y is more than or equal to 0.01 and less than or equal to 0.08, and z is more than or equal to 0.1.
Preferably, x=0.4, y=0.04 and z=0.01.
The invention provides a preparation method of the yellow fluorescent material, which comprises the following steps:
Mixing a strontium compound, a barium compound, a silicon compound, a cerium compound and a europium compound with a grinding medium, and grinding to obtain a mixed raw material;
And (3) presintering the mixed raw materials, and calcining the mixed raw materials in a protective atmosphere to obtain the yellow fluorescent material.
Preferably, the strontium compound comprises SrCO 3; the barium compound includes BaCO 3; the silicon compound includes SiO 2; the cerium compound comprises Ce 2(CO3)3 or CeO 2; the europium compound comprises Eu 2O3;
the grinding time is 10-30 min; the presintering temperature is 950-1050 ℃ and the presintering time is 0.5-1 h;
The calcining temperature is 1250-1350 ℃ and the calcining time is 4-5 h;
The protective atmosphere consists of 90-95% of nitrogen and 5-10% of hydrogen in percentage by volume.
Preferably, the yellow fluorescent material has an average particle diameter of 5 to 15 μm.
The invention provides the application of the yellow fluorescent material prepared by the technical scheme or the preparation method of the technical scheme in improving the color development performance of inorganic yellow pigment.
The invention provides a high-color-rendering inorganic yellow fluorescent pigment, which comprises yellow fluorescent powder and inorganic yellow pigment without yellow light emission;
The yellow fluorescent powder is the yellow fluorescent material prepared by the technical scheme or the preparation method; the non-yellow light emitting inorganic yellow pigment includes SrCrO 4、BiVO4 or PbCrO 4.
Preferably, the mass of the yellow fluorescent powder is 3-35% of the total mass of the yellow fluorescent powder and the inorganic yellow pigment.
The invention provides a preparation method of the inorganic yellow fluorescent pigment with high color rendering property, which comprises the following steps: and mixing the inorganic yellow pigment, the yellow fluorescent powder and water, and sequentially drying and grinding to obtain the inorganic yellow fluorescent pigment with high color rendering property.
Preferably, the mixing is performed under the condition of ultrasonic vibration, the frequency of the ultrasonic vibration is 28-40 KHz, and the time is 5-15 min; the drying temperature is 50-90 ℃ and the drying time is 1-3 h; the fineness of grinding is less than or equal to 15 mu m.
The invention provides a yellow fluorescent material, the chemical composition is Sr 2-x-y-zBaxSiO4:yCe3+,zEu2+, wherein, x is more than or equal to 0.2 and less than or equal to 1, y is more than or equal to 0.01 and less than or equal to 0.08, and z is more than or equal to 0.1. The Ce-Eu energy transfer exists in the Ce-Eu co-doped yellow fluorescent material provided by the invention: sr 2-xBaxSiO4:Ce3+ emits blue light under near ultraviolet excitation, while Sr 2-xBaxSiO4:Eu2+ emits yellow light under near ultraviolet and blue excitation, and there is a certain overlap region between the emission of Ce 3+ and the excitation of Eu 2+, which allows energy transfer between the two. According to the invention, ce ions and Eu ions are doped in the Sr 2-xBaxSiO4 system at the same time, and Ce-Eu energy transfer can occur, so that an emission spectrum has stronger emission intensity, yellow luminescence in the spectrum is obviously increased, and the luminescence intensity of the fluorescent powder is enhanced. Therefore, the yellow fluorescent material has a very wide excitation band, can be effectively excited by near ultraviolet light and blue light, has very strong absorption in a wave band of 300-450 nm, emits yellow light with a main peak of about 550nm, and has higher emission intensity.
The yellow fluorescent material is prepared by adopting a traditional high-temperature solid phase method, and the preparation process is simple and feasible, low in cost and pollution-free.
The yellow fluorescent material provided by the invention can be combined with the traditional inorganic pigment to exert potential value: the yellow fluorescent material (capable of strongly emitting visible yellow light after stimulated radiation) and the inorganic yellow pigment (both have the characteristics of high absorption of blue light and high reflection of yellow light) are combined to prepare the inorganic yellow fluorescent pigment, the addition of the yellow fluorescent material can enhance the reflection of the traditional inorganic pigment on yellow, compared with the large increase of the reflection of yellow, the addition of the novel yellow fluorescent material does not increase the reflection of blue (complementary color of yellow) of the traditional inorganic pigment, and the prepared inorganic yellow fluorescent pigment has the superposition effect of fluorescent pigment absorption-reflection light and fluorescent powder excitation-emission light in a visible light long-wave region, so that the diffuse reflection effect of the inorganic fluorescent pigment on yellow is obviously enhanced under sunlight, and the color development performance of the inorganic pigment is effectively improved.
The color development performance parameters of the inorganic yellow fluorescent pigment product prepared by the invention, such as brightness value L, yellowness value b, yellow light area reflectivity and the like, are obviously improved compared with the pure reflective pigment. The inorganic yellow fluorescent pigment has wide sources of raw materials, can expand the application range, and the doping proportion of the yellow fluorescent material is different due to the difference of the performances of the pigment and the fluorescent powder when the performance of the yellow fluorescent material is improved for other yellow inorganic pigments.
Drawings
FIG. 1 is an XRD pattern of the yellow phosphor of example 1;
FIG. 2 is a graph showing the excitation and emission spectra of the yellow phosphor of example 1;
FIG. 3 is an XRD pattern of the yellow phosphor of example 2;
FIG. 4 is a graph showing the excitation and emission spectra of the yellow phosphor of example 2;
FIG. 5 is an XRD pattern of the yellow phosphor of example 3;
FIG. 6 is a graph showing the excitation and emission spectra of the yellow phosphor of example 3;
FIG. 7 is a graph showing the emission spectra of the yellow phosphors of examples 1 to 3;
FIG. 8 is a graph showing the excitation and emission spectra of the yellow phosphors of example 3 and comparative example 1;
FIG. 9 is a graph showing the excitation and emission spectra of the phosphors of example 3 and comparative examples 1 to 2;
FIG. 10 is a graph showing excitation and emission spectra of the phosphors prepared in examples 3 to 6 and comparative examples 3 to 4;
FIG. 11 is a graph showing the reflectance spectrum of the yellow phosphor of example 3 after the yellow pigment was incorporated at different ratios.
Detailed Description
The invention provides a yellow fluorescent material, the chemical composition is Sr 2-x-y-zBaxSiO4:yCe3+,zEu2+, wherein, x is more than or equal to 0.2 and less than or equal to 1, y is more than or equal to 0.01 and less than or equal to 0.08, and z is more than or equal to 0.1.
In the present invention, x <1 is preferably 0.2.ltoreq.x, more preferably 0.3 to 0.8, still more preferably 0.4 to 0.6; preferably 0.01< y.ltoreq.0.08, more preferably 0.02 to 0.06, still more preferably 0.04 to 0.06; preferably 0< z <0.1, more preferably 0.002 to 0.01, still more preferably 0.003 to 0.006.
In the present invention, x is the mole percent of Ba relative to the substituted atom Sr, and y and z are the mole percent of Ce 3+ and Eu 2+ relative to Sr in order.
As a preferred embodiment of the present invention, x=0.4, y=0.04, and z=0.01, and the chemical composition of the corresponding yellow fluorescent material is Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+.
Proper Ba 2+ is introduced into Sr 2SiO4, so that a stable alpha' -Sr 2SiO4 phase structure can be obtained, and the strongest emission wavelength can be moved within a certain wavelength by changing the doping amount of Ba 2+; according to the invention, researches show that (Sr, ba) 2SiO4:Ce3+ emits blue light under the excitation of near ultraviolet rays, while (Sr, ba) 2SiO4:Eu2+ emits yellow light under the excitation of near ultraviolet rays and blue light, and a certain overlapping area exists between the emission of Ce 3+ and the excitation of Eu 2+, so that energy transfer can exist between the emission of Ce 3+ and the excitation of Eu 2+.
The invention provides a preparation method of the yellow fluorescent material, which comprises the following steps:
Mixing a strontium compound, a barium compound, a silicon compound, a cerium compound and a europium compound with a grinding medium, and grinding to obtain a mixed raw material;
And (3) presintering the mixed raw materials, and calcining the mixed raw materials in a protective atmosphere to obtain the yellow fluorescent material.
In the present invention, the preparation materials are commercially available as known to those skilled in the art unless otherwise specified.
In the present invention, the strontium compound preferably includes SrCO 3; the barium compound preferably comprises BaCO 3; the silicon compound preferably comprises SiO 2; the cerium compound preferably includes Ce 2(CO3)3 or CeO 2; the europium compound preferably comprises Eu 2O3;
In the present invention, the grinding medium is preferably ethanol or acetone, and the grinding time is preferably 10 to 30min, more preferably 20min; the invention has no special limit to the dosage of the grinding medium, and ensures uniform mixing according to actual requirements; in an embodiment of the invention, the volume ratio of the total mass of strontium compound, barium compound, silicon compound, cerium compound, and europium compound to the milling media is 1.5g:20mL.
In the present invention, the temperature of the pre-sintering is preferably 950 to 1050 ℃, more preferably 1000 ℃, and the time is preferably 0.5 to 1h, more preferably 1h; according to the invention, carbonate in the raw materials is decomposed by presintering, so that the shrinkage rate of the raw materials is improved, the raw materials are more closely contacted, and the solid phase reaction is more sufficient.
In the present invention, the temperature of the calcination is preferably 1250 to 1350 ℃, more preferably 1300 ℃, and the time is preferably 4 to 5 hours; the protective atmosphere preferably consists of 90-95% nitrogen and 5-10% hydrogen in volume percent.
After the calcination is completed, the obtained product is preferably cooled in air, and the obtained calcined product is ground to obtain a yellow fluorescent material; the grinding is not particularly limited, and may be carried out to a desired particle size.
In the present invention, the average particle diameter of the yellow fluorescent material is preferably 5 to 15. Mu.m, more preferably 10. Mu.m.
The invention provides the application of the yellow fluorescent material prepared by the technical scheme or the preparation method of the technical scheme in improving the color development performance of inorganic yellow pigment.
The inorganic yellow pigment is a pigment applied to paint and spray paint.
The invention provides a high-color-rendering inorganic yellow fluorescent pigment, which comprises yellow fluorescent powder and inorganic yellow pigment without yellow light emission;
The yellow fluorescent powder is the yellow fluorescent material prepared by the technical scheme or the preparation method; the non-yellow light emitting inorganic yellow pigment includes SrCrO 4、BiVO4 or PbCrO 4.
In the present invention, the mass of the yellow phosphor is preferably 3 to 35% of the total mass of the yellow phosphor and the inorganic yellow pigment, more preferably 15 to 25%.
In the present invention, the average particle diameter of the inorganic yellow pigment is preferably 1 μm or less.
The invention provides a preparation method of the inorganic yellow fluorescent pigment with high color rendering property, which comprises the following steps: and mixing the inorganic yellow pigment, the yellow fluorescent powder and water, and sequentially drying and grinding to obtain the inorganic yellow fluorescent pigment with high color rendering property.
In the present invention, the mixing is preferably performed under ultrasonic vibration, the frequency of which is preferably 28 to 40KHz, more preferably 32 to 35KHz, and the time is preferably 5 to 15min, more preferably 10min; the invention has no special limit to the water consumption, and ensures that the materials are uniformly mixed; the drying temperature is preferably 50-90 ℃, more preferably 60 ℃, and the drying time is preferably 1-3 h, more preferably 2-3 h; the fineness of the grinding is preferably 15 μm or less, more preferably 1 to 5 μm.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
The embodiment provides Sr 1.558Ba0.4SiO4:0.04Ce3+,0.002Eu2+ yellow fluorescent powder, and the preparation method thereof comprises the following steps:
(1) Weighing 0.7830g SrCO3(99.0％)、0.2758g BaCO3(99.0％)、0.2099g SiO2(99.0％)、0.0012g Eu2O3(99.99％) and 0.0322g Ce 2(CO3)3 (99.9%) as raw materials according to the stoichiometric ratio of the chemical formula Sr 1.558Ba0.4SiO4:0.04Ce3+,0.002Eu2+;
(2) Mixing all the raw materials with ethanol according to the mass to volume ratio of 1.5g to 20mL, and grinding for 20min to obtain a mixed raw material;
(3) Placing the mixed raw materials into an alumina crucible, placing the alumina crucible into a tube furnace, presintering for 1h at 1000 ℃, then heating to 1300 ℃ under a reducing atmosphere (consisting of 95% by volume of nitrogen and 5% by volume of hydrogen), calcining for 4h, removing a heating furnace body after calcining, and cooling in air to obtain a calcined product;
(4) The calcined product was ground to an average particle diameter of 10 μm to obtain yellow phosphor.
Example 2
The embodiment provides Sr 1.554Ba0.4SiO4:0.04Ce3+,0.006Eu2+ yellow fluorescent powder, and the preparation method thereof comprises the following steps:
(1) 0.7802g SrCO3(99.0％)、0.2756g BaCO3(99.0％)、0.2097g SiO2(99.0％)、0.0037g Eu2O3(99.99％) and 0.0321g Ce 2(CO3)3 (99.9%) are weighed according to the stoichiometric ratio of the chemical formula Sr 1.554Ba0.4SiO4:0.04Ce3+,0.006Eu2+ as raw materials;
(2) Mixing all the raw materials with acetone according to the mass to volume ratio of 1.5g to 20mL, and grinding for 20min to obtain a mixed raw material;
(3) Placing the mixed raw materials into an alumina crucible, placing the alumina crucible into a tube furnace, presintering for 1h at 1000 ℃, then heating to 1300 ℃ under a reducing atmosphere (consisting of 95% by volume of nitrogen and 5% by volume of hydrogen), calcining for 4h, removing a heating furnace body after calcining, and cooling in air to obtain a calcined product;
(4) The calcined product was ground to an average particle diameter of 5 μm to obtain yellow phosphor.
Example 3
The embodiment provides Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ yellow fluorescent powder, and the preparation method thereof comprises the following steps:
(1) 0.7775g SrCO3(99.0％)、0.2753g BaCO3(99.0％)、0.2096g SiO2(99.0％)、0.0061g Eu2O3(99.99％) and 0.0321g Ce 2(CO3)3 (99.9%) are weighed according to the stoichiometric ratio of the chemical formula Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ as raw materials;
(2) Mixing all the raw materials with acetone according to the mass to volume ratio of 1.5g to 20mL, and grinding for 20min to obtain a mixed raw material;
(3) Placing the mixed raw materials into an alumina crucible, placing the alumina crucible into a tube furnace, presintering for 1h at 1000 ℃, then heating to 1300 ℃ under a reducing atmosphere (consisting of 95% by volume of nitrogen and 5% by volume of hydrogen), calcining for 4h, removing a heating furnace body after calcining, and cooling in air to obtain a calcined product;
(4) The calcined product was ground to an average particle diameter of 15 μm to obtain yellow phosphor.
Comparative example 1
The comparative example provides Sr 1.59Ba0.4SiO4:0.01Eu2+ yellow fluorescent powder, and the preparation method comprises the following steps:
(1) Weighing 0.8155gSrCO3(99.0％)、0.2742g BaCO3(99.0％)、0.2087g SiO2(99.0％)、0.0061g Eu2O3(99.99％) as a raw material according to the stoichiometric ratio of the chemical formula Sr 1.59Ba0.4SiO4:0.01Eu2+;
(2) Mixing all the raw materials with acetone according to the mass to volume ratio of 1.5g to 20mL, and grinding for 20min to obtain a mixed raw material;
(3) Placing the mixed raw materials into an alumina crucible, placing the alumina crucible into a tube furnace, presintering for 1h at 1000 ℃, then heating to 1300 ℃ under a reducing atmosphere (consisting of 95% by volume of nitrogen and 5% by volume of hydrogen), calcining for 4h, removing a heating furnace body after calcining, and cooling in air to obtain a calcined product;
(4) The calcined product was ground to an average particle diameter of 15 μm to obtain yellow phosphor.
Comparative example 2
The comparative example provides Sr 1.56Ba0.4SiO4:0.04Ce3+ blue fluorescent powder, and the preparation method comprises the following steps:
(1) Weighing 0.7960gSrCO3(99.0％)、0.2728g BaCO3(99.0％)、0.2077g SiO2(99.0％)、0.0318gCe2(CO3)3(99.9％) as a raw material according to the stoichiometric ratio of the chemical formula Sr 1.56Ba0.4SiO4:0.04Ce3+;
(2) Mixing all the raw materials with acetone according to the mass to volume ratio of 1.5g to 20mL, and grinding for 20min to obtain a mixed raw material;
(3) Placing the mixed raw materials into an alumina crucible, placing the alumina crucible into a tube furnace, presintering for 1h at 1000 ℃, then heating to 1300 ℃ under a reducing atmosphere (consisting of 95% by volume of nitrogen and 5% by volume of hydrogen), calcining for 4h, removing a heating furnace body after calcining, and cooling in air to obtain a calcined product;
(4) The calcined product was ground to an average particle diameter of 15 μm to obtain blue phosphor.
Examples 4 to 6 and comparative examples 3 to 4
Phosphors of different compositions were prepared according to the formulation of table 1, according to the preparation conditions of example 3.
Table 1 raw material ratios of examples 3 to 6 and comparative examples 3 to 4
Characterization and performance testing
FIG. 1 is an XRD pattern of the yellow phosphor of example 1; FIG. 3 is an XRD pattern of the yellow phosphor of example 2; FIG. 5 is an XRD pattern of the yellow phosphor of example 3; as can be seen from fig. 1,3 and 5, the yellow luminescent materials prepared in examples 1 to 3 have good single-phase samples with diffraction peak positions that match the standard card.
The yellow phosphors prepared in example 1, example 2 and example 3 were subjected to excitation and emission tests using a fluorescence spectrophotometer, and the spectral diagrams are shown in fig. 2, fig. 4 and fig. 6, respectively. As can be seen from fig. 2, fig. 4 and fig. 6, the prepared luminescent material has an excitation peak range of 300-400 nm, the strongest excitation peak is 350nm, and can effectively absorb excitation in the near ultraviolet range. As can be seen from FIG. 2, the yellow phosphor prepared in example 1 has two emission peaks, namely, an emission peak of Ce 3+ at about 410nm and an emission peak of Eu 2+ at about 540nm, and the emission intensity Ce 3+ is greater than Eu 2+; namely, the characteristic emission peaks of Eu and Ce exist in the yellow fluorescent powder at the same time, which proves that the doping of Eu and Ce is successful; as can be seen from fig. 4 and 6, eu 2+ of the yellow phosphor prepared in example 2 has an emission intensity greater than Ce 3+, a strongest emission wavelength range is 500 to 600nm, and a strongest emission peak is located in a yellow light region of 550 nm.
In addition, as can be seen from fig. 6, in embodiment 3, the emission spectrum of Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ includes a yellow band of visible light, and the excitation peak is located in the near ultraviolet region, so that the fluorescent powder and the pigment can be effectively prevented from absorbing blue light at the same time, which indicates that the yellow fluorescent powder Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ has excellent luminescence performance. Therefore, the fluorescent pigment prepared by using the Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ fluorescent powder can be excited by sunlight outdoors, and yellow light is emitted to improve the color rendering property of the pigment.
The emission spectra of the yellow phosphors prepared in comparative example 1, example 2 and example 3 are shown in fig. 7. As can be seen from fig. 7, the yellow phosphors prepared in examples 2 and 3 have a decreased emission peak and an increased emission peak of Eu 2+ compared to the yellow phosphor Ce 3+ prepared in example 1, which demonstrates that the system enhances emission of Eu 2+ by Ce-Eu energy transfer process.
The yellow phosphors of example 3 and comparative example 1, and the blue phosphor of comparative example 2 were subjected to excitation and emission spectrum tests, and the results are shown in fig. 8 to 9. As can be seen from fig. 8 to 9, the excitation spectrum of the yellow phosphor in comparative example 1 and the emission spectrum of the blue phosphor in comparative example 2 are significantly overlapped, and compared with the excitation and emission spectra of the yellow phosphor in comparative example 1, the characteristic excitation peak of Ce 3+ also exists in the excitation spectrum of example 3, which indicates that Ce 3+ doping is successful, and the emission intensity of the yellow phosphor obtained after Ce 3 + is significantly enhanced in example 3. It was confirmed that the occurrence of Ce-Eu energy transfer enhances Eu 2+ emission.
Fig. 10 is a graph showing excitation and emission spectra of the phosphors prepared in examples 3 to 6 and comparative examples 3 to 4, and it is understood from fig. 10 that, as the Ba ion doping amount is changed from x=0 to x=1.0, the emission peak wavelength of the phosphor is blue shifted from 570nm to about 520nm, and the yellow emission and emission intensity of the phosphor Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ can be effectively adapted to the application thereof in yellow pigment at x=0.4, showing the most excellent emission performance of the phosphor.
Application example
The Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ yellow phosphor prepared in example 3 was incorporated into an inorganic yellow pigment SrCrO 4, which was specifically prepared as follows:
The Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ yellow fluorescent powder and the inorganic yellow pigment SrCrO 4 prepared in example 3 were weighed according to the mass ratios shown in table 2, respectively, to obtain inorganic yellow fluorescent pigments with different mass ratios, and specific data are shown in table 2.
TABLE 2 theoretical mass ratio of inorganic yellow fluorescent pigment (note: 1g total)
| Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ (the doping amount is set as m) | SrCrO4 |
| 0％ | 100％ |
| 15％ | 85％ |
| 20％ | 80％ |
| 25％ | 75％ |
| 30 | 70％ |
The preparation method of the inorganic yellow fluorescent pigment comprises the following steps:
Mixing Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ yellow fluorescent powder and SrCrO 4 pigment (average grain diameter is less than or equal to 1 mu m), dissolving in 5mL distilled water, ultrasonically vibrating at 32kHz for 10min to uniformly mix, drying at 60 ℃ for 3h, and grinding in a mortar to obtain the inorganic yellow fluorescent pigment with fineness of 1-5 mu m.
Test case
The inorganic yellow fluorescent pigment samples with different mass ratios in the application examples are tested by adopting a desk-top color meter, the measured samples are pressed into powder cakes in a cuvette, the samples are directly measured by adopting ultraviolet and visible light as a light source and a reflection mode, the parameter values of undoped fluorescent powder and mixed powder are compared by utilizing a comparison measurement mode, and therefore, the effect of the doped Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ powder on the SrCrO 4 yellow inorganic pigment is determined, and the result is shown in the table 3.
TABLE 3 chromaticity value data for inorganic yellow fluorescent pigments incorporating different amounts of Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ powder
| Sr1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+：SrCrO4 | L* | b* |
| 0％：100％ | 87.20 | 29.97 |
| 15％：75％ | 88.38 | 30.15 |
| 20％：80％ | 91.20 | 31.82 |
| 25％：75％ | 89.79 | 31.26 |
| 30％：70％ | 89.52 | 30.55 |
As can be seen from table 3, when the mixing ratio of Sr 1.55Ba0.4SiO4:0.04Ce3 +,0.01Eu2+ powder to SrCrO 4 pigment is 20%:80%, the brightness value L increases by 4.0%, and the effect on the color development performance parameter of the pigment is the greatest, compared with the SrCrO 4 pigment without the phosphor, which indicates that the addition of Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ powder well increases the brightness of SrCrO 4 pigment, so that it looks brighter; the yellowness value b increases by 1.85%, indicating that the inorganic pigment color is more yellow under simulated solar illumination after the fluorescent powder is doped. Based on the changes in the above data, conclusions are drawn: the SrCrO 4 pigment has obviously improved color-developing capability after being doped with Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ powder, and has the most obvious effect when the doping proportion is 20 percent.
Fig. 11 is a reflection spectrum chart of the Sr 1.55Ba0.4SiO4:0.04Ce3+,0.01Eu2+ phosphor in example 3 after being doped with the SrCrO 4 pigment in different proportions, and as can be seen from fig. 11, the incorporation of the phosphor significantly improves the reflectivity of the pigment in yellow light band, and compared with the pure SrCrO 4 pigment, the reflectivity of the pigment after being doped with 20% of the phosphor is improved by 6.8%, which effectively indicates that the addition of the phosphor can effectively improve the color rendering performance of the pigment.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. A yellow fluorescent material is characterized in that the chemical composition is Sr 2-x-y-zBaxSiO4:yCe3+,zEu2+, wherein, x is more than or equal to 0.2 and less than or equal to 1, y is more than or equal to 0.01 and less than or equal to 0.08, and z is more than or equal to 0.1.
2. The yellow fluorescent material according to claim 1, wherein x=0.4, y=0.04 and z=0.01.
3. The method for preparing a yellow fluorescent material according to claim 1 or 2, comprising the steps of:
Mixing a strontium compound, a barium compound, a silicon compound, a cerium compound and a europium compound with a grinding medium, and grinding to obtain a mixed raw material;
And (3) presintering the mixed raw materials, and calcining the mixed raw materials in a protective atmosphere to obtain the yellow fluorescent material.
4. A process according to claim 3, wherein,
The strontium compound includes SrCO 3; the barium compound includes BaCO 3; the silicon compound includes SiO 2; the cerium compound comprises Ce 2(CO3)3 or CeO 2; the europium compound comprises Eu 2O3;
the grinding time is 10-30 min; the presintering temperature is 950-1050 ℃ and the presintering time is 0.5-1 h;
The calcining temperature is 1250-1350 ℃ and the calcining time is 4-5 h;
The protective atmosphere consists of 90-95% of nitrogen and 5-10% of hydrogen in percentage by volume.
5. The method according to claim 3 or 4, wherein the yellow fluorescent material has an average particle diameter of 5 to 15 μm.
6. The yellow fluorescent material of claim 1-2 or the yellow fluorescent material prepared by the preparation method of any one of claims 3-5, and the application thereof in improving the color development performance of inorganic yellow pigment.
7. An inorganic yellow fluorescent pigment with high color rendering property, which is characterized by comprising yellow fluorescent powder and inorganic yellow pigment without yellow light emission;
The yellow fluorescent powder is the yellow fluorescent material of claims 1-2 or the yellow fluorescent material prepared by the preparation method of any one of claims 3-5; the non-yellow light emitting inorganic yellow pigment includes SrCrO 4、BiVO4 or PbCrO 4.
8. The high-color-rendering inorganic yellow fluorescent pigment according to claim 7, wherein the mass of the yellow fluorescent powder is 3 to 35% of the total mass of the yellow fluorescent powder and the inorganic yellow pigment.
9. The method for preparing the inorganic yellow fluorescent pigment with high color rendering property according to claim 7 or 8, comprising the following steps: and mixing the inorganic yellow pigment, the yellow fluorescent powder and water, and sequentially drying and grinding to obtain the inorganic yellow fluorescent pigment with high color rendering property.
10. The preparation method according to claim 9, wherein the mixing is performed under ultrasonic vibration, the frequency of the ultrasonic vibration is 28-40 KHz, and the time is 5-15 min; the drying temperature is 50-90 ℃ and the drying time is 1-3 h; the fineness of grinding is less than or equal to 15 mu m.
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