CN103834391A - Europium ion activated silicon-based nitrogen oxide green fluorescent powder and preparation method thereof - Google Patents
Europium ion activated silicon-based nitrogen oxide green fluorescent powder and preparation method thereof Download PDFInfo
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- CN103834391A CN103834391A CN201410100536.0A CN201410100536A CN103834391A CN 103834391 A CN103834391 A CN 103834391A CN 201410100536 A CN201410100536 A CN 201410100536A CN 103834391 A CN103834391 A CN 103834391A
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Abstract
The invention belongs to the technical field of a rare-earth luminescent material, and relates to europium ion activated silicon-based nitrogen oxide green fluorescent powder and a preparation method thereof. The europium ion activated silicon-based nitrogen oxide green fluorescent powder comprises chemical ingredients as shown in the following chemical formula: M3(1-x)Si2O4N2:3xEu<2+>, wherein the M element is an alkaline-earth metal element such as Ca, Mg, Sr, Ba and the like, x is not smaller than 0.002 and not larger than 0.01, and the Eu<2+> is doped rare-earth ion. The preparation method disclosed by the invention is used for synthesizing the green fluorescent powder M3(1-x)Si2O4N2:3xEu<2+> through a high-temperature solid-phase synthesis method. The green fluorescent powder emits intensive green light under excitation of near ultraviolet light; the absorbency is quite high within an excitation wavelength range of 270nm-450nm; the main emission peak is at about 510nm, and the green fluorescent powder has high luminous efficiency, high intensity and good thermal stability and can be used in white light LED (Light Emitting Diode) with high color rendering property; the preparation method of the green fluorescent powder is simple, gentle in reaction condition, easy to operate, energy-saving and time-saving, and has extremely good application prospect in solid illumination field.
Description
Technical field
The present invention relates to a kind of europium ion and activate silica-based nitrogen oxide green fluorescent powder and preparation method thereof, be particularly related to a kind of under near ultraviolet excitation the fluorescent material of transmitting green fluorescence, it can be applicable to, in ultraviolet one near ultraviolet type white light LEDs, belong to rare earth luminescent material technical field.
Background technology
White light emitting diode (LED) be called as the 4th generation lighting source, as solid light source of new generation, the shortcomings such as the energy consumption that traditional incandescent light and luminescent lamp exist is high, frangible except overcoming, pollution, also have that volume is little, environmental protection, speed of response is fast, the life-span is long, can planar package, luminous intensity high, efficient, energy-conservation, vibration resistance, low voltage drive and can not cause environmental pollution etc. to have advantage.Particularly in recent years, along with developing rapidly of blueness, purple and ultraviolet LED, make white light LEDs have very large application prospect at lighting field, be acknowledged as the green illumination light source of current replace fluorescent lamps and incandescent light.
At present, the form of acquisition white light LEDs mainly contains two kinds: one is to excite three primary colours (red, green, blue) fluorescent material, combination results white light with ultraviolet, near ultraviolet LED.Such as with Y
2o
2s:Eu
3+as rouge and powder, BaMgSiO
4as green powder, Ba
2si
3o
8as blue powder, under ultraviolet excitation, can realize white light LEDs.But because the green emitting phosphor of realizing in white light LEDs relatively lacks, luminous intensity, luminous efficiency are not high; Another kind is to use ultraviolet, near ultraviolet or blue-light LED chip to add yellow fluorescent powder, and the two light sending is mixed to form white light, the blue-light excited YAG:Ce that wherein GaN base chip is launched
3+fluorescent material is with the fastest developing speed, has realized marketization application.This method is that application is also the most ripe at most at present, but shortcoming is fairly obvious, and major cause is the white light that blue chip and gold-tinted two primary colours are compounded to form, and has lacked red composition, so colour rendering index is on the low side.These deficiencies of fluorescent material have become the bottleneck that improves white light LEDs development, the performance of fluorescent material has determined the technical indicators such as the luminous efficiency, colour temperature, colour rendering index of white light LEDs, and therefore exploitation can be become the focus of current research and urgent task by the green phosphor for white light LED of near ultraviolet excitation.
At present, nitric oxide fluorescent powder becomes the study hotspot of field of light emitting materials gradually.Nitric oxide fluorescent powder has the broadband excitation band from ultraviolet to visible region, by changing the chemical constitution of silicon-based nitrogen oxide fluorescent powder, can realize indigo plant, green, red, yellow full wavelength emission, and stability is better than the fluorescent material of other systems far away, and nitric oxide fluorescent powder synthesis condition is relatively simple, therefore the research of nitric oxide fluorescent powder is had to important scientific meaning and using value.
Summary of the invention
Technical problem to be solved by this invention is that a kind of novel preparation method of above-mentioned green emitting phosphor is provided.The simple easy handling of the method, the reaction times is short, sintering temperature is low and the light-emitting phosphor intensity of preparation is high, luminous efficiency is high, stable chemical nature, has wider wave band and the emission band etc. of exciting.
The present invention gos deep into, at length research, by controlling the factors such as chemical constitution, proportioning raw materials, has solved above-mentioned technical problem.Concrete scheme is as follows:
A kind of europium ion provided by the invention activates silica-based nitrogen oxide green fluorescent powder and preparation method thereof, and its chemical composition can be by following chemical formulation: M
3 (1-x)si
2o
4n
2: 3xEu
2+, wherein M element is one or more in Ca, Mg, Sr or Ba, 0.002≤x≤0.01.Comprise the following steps:
1. according to chemical general formula M
3 (1-x)si
2o
4n
2: 3xEu
2+calculate respectively, take reaction reagent MCO
3, purity 99.99%, SiO
2, purity 99.6%, Si
3n
4, purity 99.99%, Eu
2o
3, purity 99.99%;
2. the MCO 1. above-mentioned steps being taken
3, SiO
2, Si
3n
4, Eu
2o
3put into mortar, add appropriate alcohol, grind 30 minutes until mix;
3. be placed in crucible dry said mixture, then put into high temperature process furnances, heating and calcining heats up under reducing atmosphere;
4. will product lower the temperature after heating again, and to be cooledly to room temperature, take out, the sample of taking-up sieves through grinding, and product is put into 80～100 DEG C of dry silica-based nitrogen oxide green fluorescent powders that obtain europium doping for 2 hours of baking oven.
Described a kind of europium ion activates the preparation method of silica-based nitrogen oxide green fluorescent powder, it is characterized in that: step 3. in sintering temperature be to rise to 1300 DEG C～1500 DEG C with the heat-up rate of 5 DEG C/min～10 DEG C/min.
Described a kind of europium ion activates the preparation method of silica-based nitrogen oxide green fluorescent powder, it is characterized in that: step 3. middle reducing atmosphere is the mixed-gas atmosphere that hydrogen and nitrogen volume ratio are 0.1～0.9.
The invention has the beneficial effects as follows:
Compared with prior art, technical scheme advantage of the present invention is:
1, the substrate material that technical solution of the present invention provides, is easy to realize the reduction of trivalent rare earth ions, and this rare earth ion can stable existence in this matrix, is difficult for deliquescence.
2, the M in technical solution of the present invention
3 (1-x)si
2o
4n
2: 3xEu
2+(wherein 0.002≤x≤0.01) green fluorescent material has wider excitation area, and excitation peak is positioned at 289nm, 328nm, 368nm, 405nm, and the strongest excitation peak is positioned near 368nm.Under near ultraviolet excitation, have very wide emission band, its emission wavelength is at 450nm～650nm, and emission peak is positioned near 510nm.Also there is very strong excitation peak at blue light 460nm near zone, can coincide with the emission peak of UV-light, blue-light LED chip, can mate well LED chip.
3, compared with commercial green emitting phosphor, the preparation process of the silica-based nitrogen oxide green fluorescent powder of the present invention is simple, and product is easy to get, and without waste water and gas discharge, environmental protection, is applicable to serialization and produces.
4, acquisition fluorescent material of the present invention, in the very strong green light of near ultraviolet excitated lower transmitting, has good thermostability, color developing and granularity, and it can be satisfied with the application of near ultraviolet white light LEDs preferably.The invention provides the preparation method of this fluorescent material, its step is simple, easy handling simultaneously.
Brief description of the drawings
Fluorescent material sample Ca prepared by Fig. 1 the present invention
3 (1-x)si
2o
4n
2: 3xEu
2+xRD diffracting spectrum.
Fluorescent material sample Ca prepared by Fig. 2 the present invention
2.97si
2o
4n
2: 0.03Eu
2+exciting light spectrogram (monitoring wavelength is 510nm) and luminescent spectrum figure (excitation wavelength is 368nm).
Embodiment
Specific embodiment of the invention scheme is described below with reference to accompanying drawings.It is evident that for the person of ordinary skill of the art: in the situation that not deviating from the spirit and scope of the invention, can therefrom carry out various modifications and variations.Thereby improvement of the present invention and the variation within the scope in claims and equivalent thereof contained in the present invention.
Embodiment 1:Ca
2.985si
2o
4n
2: 0.015Eu
2+preparation
First, by chemical formula Ca
2.985si
2o
4n
2: 0.015Eu
2++stoichiometric ratio take reaction raw materials CaCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1300 DEG C, this temperature lower calcination 6 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ca of europium doping through grinding, after thermal treatment
2.985si
2o
4n
2: 0.015Eu
2+green emitting phosphor.
Embodiment 2:Ca
2.97si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Ca
2.97si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials CaCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1400 DEG C, this temperature lower calcination 8 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ca of europium doping through grinding, after thermal treatment
2.97si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Embodiment 3:Ca
2.85si
2o
4n
2: 0.15Eu
2+preparation
First, by chemical formula Ca
2.85si
2o
4n
2: 0.15Eu
2+stoichiometric ratio take reaction raw materials CaCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1500 DEG C, this temperature lower calcination 6 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ca of europium doping through grinding, after thermal treatment
2.85si
2o
4n
2: O.15Eu
2+green emitting phosphor.
Embodiment 4:Ba
2.97si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Ba
2.97si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials BaCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1500 DEG C, this temperature lower calcination 8 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ba of europium doping through grinding, after thermal treatment
2.97si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Embodiment 5:Sr
2.97si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Sr
2.97si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials SrCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1400 DEG C, this temperature lower calcination 6 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Sr of europium doping through grinding, after thermal treatment
2.97si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Embodiment 6:Mg
2.97si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Mg
2.97si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials MgCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1500 DEG C, this temperature lower calcination 8 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Mg of europium doping through grinding, after thermal treatment
2.97si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Embodiment 7:Ca
1.35mg
1.35si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Ca
1.35mg
1.35si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials CaCO
3, MgCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1400 DEG C, this temperature lower calcination 6 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ca of europium doping through grinding, after thermal treatment
2.7mg
0.27si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Embodiment 8:Ca
1.35ba
1.35si
2o
4n
2: 0.03Eu
2+preparation
First, by chemical formula Ca
1.35ba
1.35si
2o
4n
2: 0.03Eu
2+stoichiometric ratio take reaction raw materials CaCO
3, BaCO
3, SiO
2, Si
3n
4, Eu
2o
3, the above-mentioned reaction raw materials taking is put into mortar, add appropriate alcohol, grind 30min left and right until mix; Then said mixture is put into loft drier, dry being placed in crucible, put into high temperature process furnances, under the mixed gas reducing atmosphere of hydrogen and nitrogen, heat up and make calcining temperature to 1400 DEG C, this temperature lower calcination 8 hours, product is lowered the temperature again, to be cooledly to room temperature, take out, the sample of taking-up obtains the silica-based oxynitride Ca of europium doping through grinding, after thermal treatment
2.7ba
0.27si
2o
4n
2: 0.03Eu
2+green emitting phosphor.
Referring to accompanying drawing 1, it is fluorescent material sample Ca prepared by this embodiment
3 (1-x)si
2o
4n
2: 3xEu
2+xRD diffracting spectrum, adopt as seen from the figure high temperature solid phase synthesis to prepare the good europkium-activated silicon-based nitrogen oxide fluorescent powder of pure phase of series of crystallization degree, thing phase purity is higher.
Referring to accompanying drawing 2, it is fluorescent material sample Ca prepared by this embodiment 2
2.978i
2o
4n
2: 0.03Eu
2+exciting light spectrogram (monitoring wavelength is 510nm) and luminescent spectrum figure (excitation wavelength is 368nm), as can be seen from Fig., excite the scope 270～450nm of wave band, there are four excitation peaks, excitation peak wavelength is positioned at 289nm, 328nm, 368nm, 405nm, and the strongest excitation peak is positioned near 368nm.Under 368nm optical excitation, emmission spectrum is wideband spectrum, and its emission wavelength is at 450nm～650nm, and emission peak is positioned near 510nm, the green glow that emissive porwer is higher.
Claims (4)
1. europium ion activates a silica-based nitrogen oxide green fluorescent powder, it is characterized in that: its moiety is by following chemical formulation: M
3 (1-x)si
2o
4n
2: 3xEu
2+, wherein M element is one or more in Ca, Mg, Sr or Ba, 0.002≤x≤0.01.
2. a kind of europium ion according to claim 1 activates the preparation method of silica-based nitrogen oxide green fluorescent powder, it is characterized in that comprising the following steps:
1. according to chemical general formula M
3 (1-x)si
2o
4n
2: 3xEu
2+calculate respectively, take reaction reagent MCO
3, purity 99.99%, SiO
2, purity 99.6%, Si
3n
4, purity 99.99%, Eu
2o
3, purity 99.99%;
2. the MCO 1. above-mentioned steps being taken
3, SiO
2, Si
3n
4, Eu
2o
3put into mortar, add appropriate alcohol, grind 30 minutes until mix;
3. be placed in crucible dry said mixture, then put into high temperature process furnances, heating and calcining heats up under reducing atmosphere;
4. will product lower the temperature after heating again, and to be cooledly to room temperature, take out, the sample of taking-up sieves through grinding, and product is put into 80～100 DEG C of dry silica-based nitrogen oxide green fluorescent powders that obtain europium doping for 2 hours of baking oven.
3. a kind of europium ion according to claim 2 activates the preparation method of silica-based nitrogen oxide green fluorescent powder, it is characterized in that: step 3. in sintering temperature be to rise to 1300 DEG C～1500 DEG C with the heat-up rate of 5 DEG C/min～10 DEG C/min.
4. a kind of europium ion according to claim 2 activates the preparation method of silica-based nitrogen oxide green fluorescent powder, it is characterized in that: step 3. middle reducing atmosphere is the mixed-gas atmosphere that hydrogen and nitrogen volume ratio are 0.1～0.9.
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| CN104277827A (en) * | 2014-09-29 | 2015-01-14 | 中国计量学院 | Preparation method of silicon nitrogen-based blue and green fluorescent powder |
| CN105315991A (en) * | 2015-10-19 | 2016-02-10 | 杭州电子科技大学 | White-light steady-persistence fluorescent material and preparation method thereof |
| CN108956556A (en) * | 2018-05-18 | 2018-12-07 | 复旦大学 | A kind of luminescence probe and time-resolved fluorescence detection system |
| CN113249126A (en) * | 2021-05-20 | 2021-08-13 | 中国科学院长春光学精密机械与物理研究所 | Cyan mechanoluminescence material for increasing low-temperature trap quantity and preparation method and application thereof |
| CN114540015A (en) * | 2022-03-29 | 2022-05-27 | 陕西师范大学 | Wide-spectrum yellow-green emitting nitrogen oxide fluorescent powder and preparation method thereof |
| CN114752383A (en) * | 2022-03-31 | 2022-07-15 | 陕西师范大学 | La2Ca3Si4N4O8Crystal, fluorescent powder and preparation method |
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Cited By (10)
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|---|---|---|---|---|
| CN104277827A (en) * | 2014-09-29 | 2015-01-14 | 中国计量学院 | Preparation method of silicon nitrogen-based blue and green fluorescent powder |
| CN104277851A (en) * | 2014-10-31 | 2015-01-14 | 重庆理工大学 | Silicate green emitting phosphor and preparation method thereof |
| CN105315991A (en) * | 2015-10-19 | 2016-02-10 | 杭州电子科技大学 | White-light steady-persistence fluorescent material and preparation method thereof |
| CN108956556A (en) * | 2018-05-18 | 2018-12-07 | 复旦大学 | A kind of luminescence probe and time-resolved fluorescence detection system |
| CN113249126A (en) * | 2021-05-20 | 2021-08-13 | 中国科学院长春光学精密机械与物理研究所 | Cyan mechanoluminescence material for increasing low-temperature trap quantity and preparation method and application thereof |
| CN113249126B (en) * | 2021-05-20 | 2023-08-15 | 中国科学院长春光学精密机械与物理研究所 | Cyan-induced luminescent material capable of increasing number of low-temperature traps, and preparation method and application thereof |
| CN114540015A (en) * | 2022-03-29 | 2022-05-27 | 陕西师范大学 | Wide-spectrum yellow-green emitting nitrogen oxide fluorescent powder and preparation method thereof |
| CN114540015B (en) * | 2022-03-29 | 2023-08-22 | 陕西师范大学 | Fluorescent powder capable of emitting nitrogen oxides in broad-spectrum yellow-green color and preparation method thereof |
| CN114752383A (en) * | 2022-03-31 | 2022-07-15 | 陕西师范大学 | La2Ca3Si4N4O8Crystal, fluorescent powder and preparation method |
| CN114752383B (en) * | 2022-03-31 | 2023-09-01 | 陕西师范大学 | La 2 Ca 3 Si 4 N 4 O 8 Crystal and fluorescent powder and preparation method thereof |
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Application publication date: 20140604 |