CN115011341B - Fluorescent powder capable of emitting broadband green light and preparation method thereof - Google Patents
Fluorescent powder capable of emitting broadband green light and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of material science, and discloses fluorescent powder capable of emitting broadband green light and a preparation method thereof. The broadband green light emitting luminescent material is prepared by La 2 W 2 O 9 Is matrix, bismuth ion is used as activator, and lutetium is doped to enhance luminous intensity, and the component is (La 1‑x‑y Lu y Bi x ) 2 W 2 O 9 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.1-10% and y is less than or equal to 30%. The invention can be effectively excited by 350nm ultraviolet light, is well matched with the wavelength of an ultraviolet LED chip, is favorable for commercialization, and has wide excitation range, and the excitation peak is broadband. The emission is broadband green light emission, the half-width is 150-340nm, the emission band well covers blue light (490 nm) lacking in the traditional illumination fluorescent powder, and the blue light gap is filled, so that the fluorescent powder has good application in full spectrum illumination. The method can be prepared by adopting a traditional high-temperature solid-phase method or a liquid-phase method, the traditional high-temperature solid-phase method is easy to commercialize, and the liquid-phase method can optimize the microcosmic appearance.
Description
Technical Field
The invention belongs to the technical field of material science, and relates to fluorescent powder capable of emitting broadband green light and a preparation method thereof.
Background
Compared with traditional incandescent lamps and other light sources, the new generation of solid-state lighting light sources, namely white Light Emitting Diodes (LEDs), has the advantages of high luminous efficiency, long service life, low energy consumption, green environmental protection and the like, and has wide application in the field of warm white light LEDs.
The most common method of manufacturing white LEDs today is to use yellow-emitting Y 3 Al 5 O 12 :Ce 3+ (YAG:Ce 3+ ) The blue InGaN chip is covered by the fluorescent powder, so that white light output is realized, but the yellow fluorescent powder and the blue chip have a small spectrum range, so that the generated white light lacks of red spectrum components, and the color rendering index of the white light LEDs is low and the color temperature is high. Thus based on YAG: ce 3+ The white LEDs produced are not well suited for indoor general lighting and there is a need to develop a warm white LEDs with a high color rendering index.
Full spectrum LEDs improve spectral continuity and color gamut saturation, making them ideal applications for high quality light sources, including photography, art houses, backlights, and the like. LEDs must overcome the blue gap (480-520 nm) to achieve full spectrum illumination similar to solar light. While phosphors that emit cyan light can compensate for the cyan light gap, they are generally poor in thermal and structural stability or low in luminous efficiency, such as BaLa 2 Si 2 S 8 :Ce 3+ La and La 3 Br(SiS 4 ) 2 :Ce 3+ . In addition, the mixing of multiple phosphors also increases the complexity of the preparation and has reabsorption phenomena, so simply preparing a cyan-emitting phosphor is not the most effective method for solving the "cyan gap" in the illumination field.
The existing green emitting fluorescent powder has unstable chemical property under blue light and low excitation efficiency as (Ba, sr) 2 SiO 4 :Eu 2+ The defects of high raw material price, inability to well cover blue light gaps and the like are greatly limited in application and are not well applicable to full spectrum illumination.
The performance of LEDs depends on the luminous performance of fluorescent powder to a great extent, and a broadband green fluorescent powder which covers blue light and green light areas is developed to solve the problem of green light gap well, so that full spectrum illumination is realized.
Disclosure of Invention
Aiming at the problems of lack of broadband green light fluorescent powder, blue light gap and the like in the field of illumination, the invention provides a tungstate fluorescent powder which takes bismuth ions as an activator and emits broadband green light and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a broad-band green light-emitting material prepared from La 2 W 2 O 9 Is matrix, bismuth ion is used as activator, and lutetium is doped to enhance luminous intensity, and the component is (La 1-x-y Lu y Bi x ) 2 W 2 O 9 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.1-10% and y is less than or equal to 30%.
The preparation method of the broadband green light emitting material can adopt a high-temperature solid-phase preparation method or a liquid-phase preparation method.
The high-temperature solid phase preparation method of the broadband green light emitting material comprises the following steps:
(1) Mixing the raw materials: the rare earth raw material can be oxide or hydroxide or nitrate; the raw material of bismuth is oxide, and tungsten and molybdenum sources are ammonium salts. The raw materials are calculated according to the stoichiometric ratio, and the raw materials of La are calcined for 1-6 hours in the air atmosphere at 600-1200 ℃ before being used. All the raw materials were mixed in an agate mortar.
(2) Grinding and mixing: adding 1-2ml of alcohol into the mixed raw material in the step (1), grinding for 30-60min, and uniformly mixing to obtain mixed powder.
(3) Calcining: calcining the mixed powder obtained in the step (2), wherein the calcining temperature is 1100-1300 ℃, the heating speed is 1-10 ℃/min, the heat preservation time is 1-10h, and the atmosphere is air.
The liquid phase preparation method of the broadband green light emitting material comprises the following steps:
(1) Liquid phase raw material reaction: the rare earth raw material is rare earth nitrate (0.2 mol/L), or rare earth oxide is taken as raw material and nitric acid is used for dissolving to obtain rare earth nitrate; the bismuth source is bismuth nitrate particles which are prepared into nitrate solution under the acidic condition, and attention is paid to the fact that the bismuth nitrate particles can not be directly dissolved in water but dissolved in dilute nitric acid in the preparation process. The tungsten source is sodium tungstate, and sodium tungstate particles are dissolved into sodium tungstate solution (0.2 mol/L); the concentrated aqueous ammonia was prepared as 0.1mol/L of dilute aqueous ammonia. Firstly, raw materials are measured according to the ratio of tungstic acid to rare earth of 1:1. Adding rare earth nitrate into the sodium tungstate solution, and uniformly stirring for 30min.
(2) Adjusting the pH: the pH of the solution obtained in step (1) was adjusted to ph=9-10 using ammonia water, and then stirring was continued for 10min.
(3) Hydrothermal reaction: pouring the reaction solution in the step (2) into a reaction kettle, and putting into a baking oven for reaction for 6-48h at 100-220 ℃.
(4) And (3) centrifuging: after cooling to room temperature, the hydrothermal product was collected by centrifugation, washed four times with deionized water, once with alcohol, and then dried at 50-95 ℃ for 12-48 hours in the atmosphere of air.
(5) Calcining: calcining the mixed powder obtained in the step (4). The calcination temperature is 1100-1300 ℃, the heating speed is 1-10 ℃/min, the heat preservation time is 1-10h, and the atmosphere is air.
The beneficial effects of the invention are as follows:
1) Can be effectively excited by 350nm ultraviolet light, is well matched with the wavelength of a commercial ultraviolet LED chip, is favorable for commercialization, and has wide excitation range, and the excitation peak is broadband.
2) The emission is broadband green light emission, the half-width is 150-340nm, the emission band well covers blue light (490 nm) lacking in the traditional illumination fluorescent powder, and the blue light gap is filled, so that the fluorescent powder has good application in full spectrum illumination.
3) Bismuth ion is used as activator, and conventional Eu is not used 2+ 、Ce 3+ The rare earth ion is used as an activator, so that the price is low, the resources are rich, and the broadband green light emission can be realized without adjusting the price state and calcining in the air. Eu (Eu) 2+ 、Ce 3 + Calcination under a reducing atmosphere is required for valence state control.
4) The method can be prepared by adopting a traditional high-temperature solid-phase method or a liquid-phase method, the traditional high-temperature solid-phase method is easy to commercialize, and the liquid-phase method can optimize the microcosmic appearance.
Drawings
Figure 1 is an XRD pattern of example 1 of the present invention.
FIG. 2 is an excitation spectrum of example 1 of the present invention.
FIG. 3 is an emission spectrum of example 1 of the present invention.
Figure 4 is an XRD pattern of example 2 of the present invention.
FIG. 5 is an excitation spectrum of example 2 of the present invention.
Fig. 6 is an emission spectrum of example 2 of the present invention.
FIG. 7 is an excitation spectrum of example 3 of the present invention.
FIG. 8 is an emission spectrum of example 3 of the present invention.
Fig. 9 is a scanning electron microscope picture of example 3 of the present invention.
FIG. 10 is an excitation spectrum of example 4 of the present invention.
FIG. 11 is an emission spectrum of example 4 of the present invention.
Fig. 12 is a scanning electron microscope picture of example 4 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings and technical schemes.
The chemical reagents used in the examples of the invention are all analytically pure grade products; XRD analysis was performed using RINT2200V/PC type X-ray diffractometer from Rigaku corporation, japan; analyzing photoluminescence performance of the sample by using a Edinburgh FLS 1000 type fluorescence spectrometer; the microscopic morphology of the sample was analyzed using an S-5000 field emission scanning electron microscope from Hitachi, japan.
EXAMPLE 1 preparation by solid phase method (La 0.98 Bi 0.02 ) 2 W 2 O 9
(1) The raw materials are weighed, and the rare earth raw materials are lanthanum oxide, bismuth oxide (bismuth is calculated according to lanthanum occupation, doping amount is calculated according to 2 percent) and ammonium tungstate. The raw materials are first calculated according to the stoichiometric ratio, and the lanthanum oxide used is calcined for 1h in an air atmosphere at 1200 ℃ before use. All weighed raw materials were mixed in an agate mortar.
(2) Grinding and mixing: adding 1ml of alcohol into the powder raw materials mixed in the step (1), grinding for 30min, and uniformly mixing.
(3) Calcining: calcining the mixed powder obtained in the step (2). Calcination temperatureThe temperature is 1300 ℃, the heating speed is 5 ℃/min, the heat preservation time is 5h, and the atmosphere is air. Cooling to room temperature with furnace after heat preservation is finished to obtain (La) 0.98 Bi 0.02 ) 2 W 2 O 9 。
EXAMPLE 2 preparation by solid phase method (La 0.75 Lu 0.24 Bi 0.01 ) 2 W 2 O 9
(1) The raw materials are weighed, and the rare earth raw materials are lanthanum oxide, bismuth oxide (calculated according to lanthanum occupation, doping amount is calculated according to 1 percent), lutetium oxide (calculated according to lanthanum replacement, replacement amount is 24 percent) and ammonium tungstate. The raw materials were first calculated in stoichiometric proportions and the lanthanum oxide used was calcined in an air atmosphere at 600 ℃ for 4 hours before use. All weighed raw materials were mixed in an agate mortar.
(2) Grinding and mixing: adding 1.5ml of alcohol into the powder raw materials mixed in the step (1), grinding for 50min, and uniformly mixing.
(3) Calcining: calcining the mixed powder obtained in the step (2). The calcination temperature is 1200 ℃, the heating speed is 1 ℃/min, the heat preservation time is 2h, and the atmosphere is air. Cooling to room temperature with furnace after heat preservation is finished to obtain (La) 0.75 Lu 0.24 Bi 0.01 ) 2 W 2 O 9 。
Example 3 liquid phase preparation
(1) Lanthanum nitrate, lutetium nitrate, bismuth nitrate and ammonium tungstate are used as raw materials, and firstly, the following steps are adopted: the ratio of (rare earth and bismuth) is 1:1, 30ml of ammonium tungstate, 0.3ml of bismuth nitrate, 22.5ml of lanthanum nitrate and 7.2ml of lutetium nitrate are taken. The nitrate was added to the sodium tungstate solution and stirred uniformly for 30min.
(2) Adjusting the pH: the pH of the solution obtained in step (1) was adjusted to ph=9 using ammonia water, and then stirring was continued for 10min.
(3) Hydrothermal reaction: pouring the reaction solution in the step (2) into a reaction kettle, and putting into a baking oven for reaction at 100 ℃ for 24 hours.
(4) And (3) centrifuging: after cooling to room temperature, the hydrothermal product was collected by centrifugation, washed four times with deionized water, once with alcohol, and then dried at 70 ℃ for 24 hours in the atmosphere of air.
(5) Calcining: calcining the mixed powder obtained in the step (4). The calcination temperature is 1300 ℃, the heating speed is 5 ℃/min, the heat preservation time is 4 hours, and the atmosphere is air. Cooling to room temperature with furnace after heat preservation is finished to obtain (La) 0.75 Lu 0.24 Bi 0.01 ) 2 W 2 O 9 The product is obtained.
Example 4 liquid phase preparation
(1) Lanthanum nitrate, lutetium nitrate, bismuth nitrate and ammonium tungstate are used as raw materials, and firstly, the following steps are adopted: the ratio of (rare earth and bismuth) is 1:1, 30ml of ammonium tungstate, 0.3ml of bismuth nitrate, 26.7ml of lanthanum nitrate and 3ml of lutetium nitrate are taken. The nitrate was added to the sodium tungstate solution and stirred uniformly for 30min.
(2) Adjusting the pH: the pH of the solution obtained in step (1) was adjusted to ph=9.5 using ammonia water, and then stirring was continued for 10min.
(3) Hydrothermal reaction: pouring the reaction solution in the step (2) into a reaction kettle, and putting into an oven to react for 24 hours at 150 ℃.
(4) And (3) centrifuging: after cooling to room temperature, the hydrothermal product was collected by centrifugation, washed four times with deionized water, once with alcohol, and then dried at 70 ℃ for 24 hours in the atmosphere of air.
(5) Calcining: calcining the mixed powder obtained in the step (4). The calcination temperature is 1200 ℃, the temperature rising speed is 5 ℃/min, the heat preservation time is 4 hours, and the atmosphere is air. Cooling to room temperature with furnace after heat preservation is finished to obtain (La) 0.89 Lu 0.10 Bi 0.01 ) 2 W 2 O 9 The product is obtained.
Claims (3)
1. A luminescent material for emitting broad band green light is prepared from La 2 W 2 O 9 Is matrix, bismuth ion is used as activator, and lutetium is doped to enhance luminous intensity, and the component is (La 1-x-y Lu y Bi x ) 2 W 2 O 9 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x=0.1-10% and y is less than or equal to 30%.
2. A high temperature solid phase preparation method of a broadband green light emitting luminescent material according to claim 1, comprising the steps of:
(1) Mixing the raw materials: the rare earth raw material is oxide or hydroxide or nitrate; the raw material of bismuth is oxide, and tungsten and molybdenum sources are ammonium salts; calculating the raw material amount according to the stoichiometric ratio, wherein the raw material of La is 600-1200 before use o Calcining 1-6h in the air atmosphere for use; mixing all the raw materials in an agate mortar;
(2) Grinding and mixing: adding alcohol 1-2ml into the mixed raw material in the step (1), grinding for 30-60min, and uniformly mixing to obtain mixed powder;
(3) Calcining: calcining the mixed powder obtained in the step (2) at 1100-1300 o C, the temperature rising speed is 1-10 o C/min, the heat preservation time is 1-10h, and the atmosphere is air.
3. A liquid phase preparation method of a broadband green light emitting luminescent material according to claim 1, characterized by comprising the steps of:
(1) Liquid phase raw material reaction: the rare earth raw material is rare earth nitrate 0.2mol/L, or rare earth oxide is taken as raw material and is dissolved by nitric acid to obtain rare earth nitrate; bismuth source is bismuth nitrate particles, which are prepared into nitrate solution under the acidic condition, and the bismuth nitrate particles cannot be directly dissolved in water in the preparation process, but are dissolved in dilute nitric acid; the tungsten source is sodium tungstate, and sodium tungstate particles are dissolved into 0.2mol/L sodium tungstate solution; preparing 0.1mol/L dilute ammonia water from the concentrated ammonia water; firstly, raw materials are measured according to the proportion of tungstic acid to rare earth of 1:1; adding rare earth nitrate into the sodium tungstate solution, and uniformly stirring for 30 min;
(2) Adjusting the pH: adjusting the pH value of the solution obtained in the step (1) to pH=9-10 by using ammonia water, and then continuing stirring for 10 min;
(3) Hydrothermal reaction: pouring the reaction solution in the step (2) into a reaction kettle, and putting into a baking oven for reaction at 100-220 ℃ for 6-48 h;
(4) And (3) centrifuging: cooling to room temperature, centrifuging to collect hydrothermal product, washing with deionized water four times, washing with ethanol once, and drying at 50-95deg.C for 12-48h under air;
(5) Calcining: calcining the mixed powder obtained in the step (4); the calcination temperature is 1100-1300 ℃, and the temperature rising speed is 1-10 o C/min, the heat preservation time is 1-10h, and the atmosphere is air.
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