CN102994075A - Silicon-based nitrogen oxide green phosphor - Google Patents

Silicon-based nitrogen oxide green phosphor Download PDF

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Publication number
CN102994075A
CN102994075A CN2012105640698A CN201210564069A CN102994075A CN 102994075 A CN102994075 A CN 102994075A CN 2012105640698 A CN2012105640698 A CN 2012105640698A CN 201210564069 A CN201210564069 A CN 201210564069A CN 102994075 A CN102994075 A CN 102994075A
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equal
nitrogen oxide
light
green phosphor
silicon
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周有福
黄得财
许文涛
洪茂椿
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

The invention provides a series of silicon-based nitrogen oxide green phosphor activated by europium, and a preparation method thereof; the chemical formula of the silicon-based nitrogen oxide green phosphor is M1-xSiyOzN ((2/3)x+(4/3)y-(2/3)z): xEu<2+>, wherein M is alkaline-earth metal element such as Mg, Ca, Sr, Ba or the like, x is more than or equal to 0.7 and less than or equal to 1.3, y is more than or equal to 2.7 and less than or equal to 2.3, z is more than or equal to 3.7 and less than or equal to 4.3, and the europium ion doping concentration range is x which is more than or equal to 0.02 and less than or equal to 0.12. The silicon-based nitrogen oxide green phosphor is simple in preparation technology and mild in reaction conditions, emits strong green light when being activated by ultraviolet light and blue light, is good in stability and high in fluorescence intensity, thus being a good white light LED green phosphor material.

Description

A kind of silica-based nitrogen oxide green fluorescent powder
Technical field
The present invention relates to rare earth luminescent material and solid-state illumination technical field, especially relate to a kind of silica-based nitrogen oxide green fluorescent powder and preparation method thereof.
Background technology
White light LEDs is as a kind of novel solid state light emitter, compare with light sources such as luminescent lamps with traditional incandescent light, it has environmental protection, energy-conservation, efficient, the response advantage such as fast, be described as after incandescent light, luminescent lamp and high-voltage gas discharging light three large light sources the 4th generation green light source.In led light source, the performance of fluorescent material has determined the technical indicators such as luminous efficiency, colour rendering index, colour temperature and work-ing life of LED, and therefore, fluorescent material has very important status in white light LEDs, is subject to extensive concern.
At present, the main path that realizes white light LEDs is the fluorescent material transformation approach, the method is by with block semiconductor chip and a phosphor combination, utilize the short wavelength's that semi-conductor chip sends light as the excitation light source of fluorescent material, excite the fluorescent material that is coated on the chip, fluorescent material is with all or part of visible light that is converted into of the luminous energy of its absorption, and realizing white light with the combination of the utilizing emitted light of chip, this method is write as pc-LED (phosphor-convered light emtting diode) usually.The fluorescent material transformation approach can be divided into two classes again according to the chip difference of using, one class is the blue chip excitated type: take blue-light LED chip as excitation light source, excitation-emission goes out the fluorescent material of gold-tinted, gold-tinted does not have absorbed blue light combination to obtain white light with part, excites YAG:Ce such as present the most frequently used blue chip 3+Yellow fluorescent powder is realized white light, perhaps excite green and red fluorescence powder with blue chip, unabsorbed blue light and green powder and rouge and powder combination realize white light, but blue chip excites yellow fluorescent powder to realize that white light LEDs lacks red light portion, be difficult for realizing low colour temperature, colour rendering index is on the low side.Another kind of is purple light or UV-light chip excitated type: excite three primary colours (red, green, blue) fluorescent material with purple light/ultraviolet leds, combination realizes white light.As with Y 2O 2S:Eu 3+As rouge and powder, Ba 2Si 3O 8: Eu 2+As blue powder, BaMgSiO 4: Eu 2+As green powder, under exciting, the ultraviolet chip can realize white light LEDs.Be used at present realizing that the central green emitting phosphor of RGB three primary colors fluorescent powder of white light LEDs relatively lacks, luminous efficiency is undesirable.
In recent years, nitride and nitric oxide fluorescent powder become the study hotspot of field of light emitting materials gradually.The primary structure of nitride/nitric oxide fluorescent powder is based on crosslinked Si 3N 4Tetrahedral network, owing to have large crystal field splitting energy and electronic cloud diffusional effect, can effectively reduce the 5d electron energy state of doping with rare-earth ions, therefore, nitride/nitric oxide fluorescent powder has the broadband excitation band from the ultraviolet to the visible region, by changing the chemical constitution of silica-based nitride/nitric 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.The synthesis condition of Nitride phosphor is relatively harsher, and synthetic cost is higher.With respect to Nitride phosphor, the synthesis condition of nitric oxide fluorescent powder is relatively gentle, therefore, the research of nitrogen oxide green fluorescent powder is had important scientific meaning and using value.Summary of the invention
The object of the invention is to provide a kind of nitric oxide fluorescent powder preparation method of gentleness, and the synthesis condition of this green emitting phosphor is simple, luminous efficiency is high, good stability, have wide exciting and emission band.
Purpose of the present invention is achieved through the following technical solutions:
A kind of silica-based oxynitride is the fluorescent material of matrix, and the chemical structural formula of described fluorescent material is:
M 1-xSi yO zN ((2/3) x+ (4/3) y-(2/3) z): xEu 2+, wherein the M element is Mg, Ca, Sr, the alkali earth metals such as Ba, 0.02≤x≤0.20,2.7≤y≤2.3,3.7≤z≤4.3.Described material can mix Mn 2+, Ce 3+, Bi 3+, Gd 3+Or Tb 3+In one or more ions, regulate excitation spectrum and emmission spectrum.
A kind of preparation method of silica-based nitrogen oxide green fluorescent powder may further comprise the steps:
1. the primitive reaction thing is: the raw material of alkaline-earth metal can use nitride M 3N 2, alkaline-earth oxide MO, alkaline earth carbonate MCO 3, alkaline earth oxalate MC 2O 4Perhaps alkaline earth hydroxide M (OH) 2And fluorochemical MF2, muriate MCl 2Deng.And SiO can be used in the silicon source 2, Si 3N 4, Si (NH) 2, SiF 4Deng raw material.
2. according to the chemical constitution of material, take by weighing by stoichiometric ratio, for example with MCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) be raw material, undertaken by following reaction formula during batching:
(2-2x)MCO 3+Si 3N 4+3SiO 2+xEu 2O 3+xH 2→2M 1-xEu xS i3O 4N 2+(2-2x)CO 2↑+xH 2O↑
3. mix the silicon-based nitrogen oxide fluorescent powder of europium by the high temperature solid phase synthesis preparation.The concrete steps of high temperature solid phase synthesis are as follows: the reaction raw materials that will take by weighing is poured in the mortar, fully is ground to mix, and changes over to after the drying in the high-temperature crucibles, puts into high temperature process furnances, passes into 5%H 2/ 95%N 2Reducing atmosphere, again cooling after the heating that heats up under normal pressure is to be cooledly taken out to room temperature; The sample that takes out obtains mixing the silica-based nitrogen oxide green fluorescent powder of europium through grinding.
4. in the above-mentioned steps, the heating schedule of described high temperature process furnances is that the heat-up rate with 5 ℃/min ~ 10 ℃/min rises to 1300 ℃ ~ 1500 ℃, insulation is 2-8 hour under this temperature, the atmosphere flow is 100 ml/min, then be cooled to 250 ℃, naturally cool to again room temperature with 5 ℃/min ~ 8 ℃/min cooling rate.
5. silica-based nitrogen oxide fluorescent material of the present invention can be used as the green emitting phosphor material of white light LEDs.
The present invention has following features:
The present invention adopts high temperature solid phase synthesis to prepare the good pure phase of series of crystallization degree to mix the europium silicon-based nitrogen oxide fluorescent powder.Fig. 1 has shown wherein Ba 0.94Si 3O 4N 2: 0.06Eu 2+The XRD diffracting spectrum of green emitting phosphor; It has very wide emission band, and its emission wavelength is in 480 nm ~ 600 nm scopes, and its emission peak is near 525 nm, and luminous intensity is high, and color developing is good, and Fig. 2 has shown its emmission spectrum under 365 nm excite.It also has very wide excitation band, and its excitation wavelength is in 270 nm ~ 500 nm scopes, and the strongest excitation peak is positioned near the 365nm, at blue light 465 nm near zones very strong excitation peak is arranged, and is identical with the emission peak of LED blue light, UV-light chip, so Ba 0.94Si 3O 4N 2: 0.06Eu 2+Fluorescent material can fine coupling led chip.
The invention provides a kind of preparation method of silica-based nitrogen oxide green fluorescent powder, its technique is simple, mild condition, production cost are lower.
Description of drawings
Ba in Fig. 1 example 2 of the present invention 0.94Si 3O 4N 2: 0.06Eu 2+The XRD diffracting spectrum of green emitting phosphor shows that its phase purity is high.
Ba in Fig. 2 example 2 of the present invention 0.94Si 3O 4N 2: 0.06Eu 2+Excitation spectrum (the λ of green emitting phosphor Em=525 nm) and emmission spectrum (λ Ex=365 nm), the strong green glow of emission.
Embodiment
Example 1
Press chemical formula Ba 0.98Eu 0.02Si 3O 4N 2Stoichiometric, accurately take by weighing BaCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material, undertaken by following reaction formula during batching:
1.96BaCO 3+Si 3N 4+3SiO 2+0.02Eu 2O 3+0.02H 2→2Ba 0.98Eu 0.02S i3O 4N 2+1.96CO 2↑+0.02H 2O↑
With the above-mentioned raw material that takes by weighing in agate mortar, add an amount of alcohol, grind about 30 min until mix, afterwards, put into 80 ℃ of drying 4 h of loft drier, in the BN crucible of then packing into, putting into high temperature process furnances heats, heat-up rate with 5 ℃/min rises to 1300 ℃, and insulation calcination 6 hours under this temperature is taken out sample after being cooled to room temperature again.The sample that takes out is ground to form the uniform powder of fineness again in agate mortar, obtain to mix the silica-based oxynitride Ba of europium 0.98Eu 0.02Si 3O 4N 2Green emitting phosphor.
Example 2
Press chemical formula Ba 0.94Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing BaCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.With the above-mentioned raw material that takes by weighing in agate mortar, after adding an amount of alcohol, grind about 30 min until mix, afterwards, put into 80 ℃ of drying 4 h of loft drier, in the BN crucible of then packing into, putting into high temperature process furnances heats, heat-up rate with 10 ℃/min rises to 1300 ℃, and insulation calcination 6 hours under this temperature is taken out sample after being cooled to room temperature again.The sample that takes out is ground to form the uniform powder of fineness again in agate mortar, obtain to mix the silica-based oxynitride Ba of europium 0.94Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 3
Press chemical formula Ba 0.90Eu 0.10Si 3O 4N 2Stoichiometric, accurately take by weighing respectively BaCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 1 and example 2.The heating schedule of high temperature process furnances is, rises to 1300 ℃ with the heat-up rate of 8 ℃/min, and the insulation calcination is 6 hours under this temperature, takes out sample after being cooled to room temperature again.The sample that takes out is ground to form the uniform powder of fineness again in agate mortar, obtain to mix the silica-based oxynitride Ba of europium 0.90Eu 0.10Si 3O 4N 2Green emitting phosphor.
Example 4
Press chemical formula Ca 0.94Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively CaCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 1 and example 3.The heating schedule of high temperature process furnances is, rises to 1500 ℃ with the heat-up rate of 5 ℃/min, and the insulation calcination is 3 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powdered sample of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Ca that mixes europium 0.94Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 5
Press chemical formula Sr 0.94Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively SrCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 7.The heating schedule of high temperature process furnances is, rises to 1400 ℃ with the heat-up rate of 5 ℃/min, and the insulation calcination is 8 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powder of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Sr that mixes europium 0.94Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 6
Press chemical formula Mg 0.94Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively MgCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 7 and example 8.The heating schedule of high temperature process furnances is, rises to 1300 ℃ with the heat-up rate of 5 ℃/min, and the insulation calcination is 4 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powder of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Mg that mixes europium 0.94Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 7
Press chemical formula Ca 0.90Ba 0.04Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively CaCO 3(99.99%), BaCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 7 and example 8.The heating schedule of high temperature process furnances is, rises to 1500 ℃ with the heat-up rate of 5 ℃/min ~ 10 ℃/min, and the insulation calcination is 5 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powder of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Ca that mixes europium 0.90Ba 0.04Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 8
Press chemical formula Ca 0.84Sr 0.10Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively CaCO 3(99.99%), SrCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 7 and example 8.The heating schedule of high temperature process furnances is, rises to 1400 ℃ with the heat-up rate of 10 ℃/min, and the insulation calcination is 6 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powder of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Ca that mixes europium 0.84Sr 0.10Eu 0.06Si 3O 4N 2Green emitting phosphor.
Example 9
Press chemical formula Ba 0.90Sr 0.04Eu 0.06Si 3O 4N 2Stoichiometric, accurately take by weighing respectively BaCO 3(99.99%), SrCO 3(99.99%), SiO 2(99.5%), Si 3N 4(99.9%), Eu 2O 3(99.99%) raw material adopts example 1 similar reaction formula to carry out during batching.The raw material that takes by weighing is processed according to example 7 and example 8.The heating schedule of high temperature process furnances is, rises to 1300 ℃ ~ 1500 ℃ with the heat-up rate of 5 ℃/min ~ 10 ℃/min, and the insulation calcination is 6 hours under this temperature, takes out sample after being cooled to room temperature again.The slight uniform powder of rear acquisition fineness that grinds of the sample that takes out namely gets the silica-based oxynitride Ba that mixes europium 0.90Sr 0.04Eu 0.06Si 3O 4N 2Green emitting phosphor.

Claims (2)

1. green emitting phosphor take silica-based oxynitride as matrix, its chemical formula is: M 1-xSi yO zN ((2/3) x+ (4/3) y-(2/3) z): xEu 2+, wherein the M element is one or more among Mg, Ca, Sr or the Ba, 0.02≤x≤0.20,2.7≤y≤2.3,3.7≤z≤4.3, and europium ion-doped concentration range is x.
2. fluorescent material according to claim 1, it is characterized in that: described material can mix Mn 2+, Ce 3+, Bi 3+, Gd 3+Or Tb 3+In one or more ions.
CN2012105640698A 2012-12-21 2012-12-21 Silicon-based nitrogen oxide green phosphor Pending CN102994075A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474829A (en) * 2017-07-18 2017-12-15 中国计量大学 A kind of high temperature resistant green emitting phosphor and its preparation method and application
CN108893107A (en) * 2018-06-21 2018-11-27 东台市天源光电科技有限公司 A kind of nitride red fluorescent powder and preparation method thereof
CN111100634A (en) * 2019-12-25 2020-05-05 武汉工程大学 Long-afterglow fluorescent material and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005154611A (en) * 2003-11-27 2005-06-16 National Institute For Materials Science Method for producing sialon fluorescent substance
JP2007223864A (en) * 2006-02-24 2007-09-06 Matsushita Electric Ind Co Ltd Oxynitride, oxynitride phosphor and light emitting device using the oxynitride phosphor
US20080296596A1 (en) * 2007-05-30 2008-12-04 Anant Achyut Setlur Novel green emitting phosphors and blends thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005154611A (en) * 2003-11-27 2005-06-16 National Institute For Materials Science Method for producing sialon fluorescent substance
JP2007223864A (en) * 2006-02-24 2007-09-06 Matsushita Electric Ind Co Ltd Oxynitride, oxynitride phosphor and light emitting device using the oxynitride phosphor
US20080296596A1 (en) * 2007-05-30 2008-12-04 Anant Achyut Setlur Novel green emitting phosphors and blends thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107474829A (en) * 2017-07-18 2017-12-15 中国计量大学 A kind of high temperature resistant green emitting phosphor and its preparation method and application
CN107474829B (en) * 2017-07-18 2020-07-17 中国计量大学 High-temperature-resistant green fluorescent powder and preparation method and application thereof
CN108893107A (en) * 2018-06-21 2018-11-27 东台市天源光电科技有限公司 A kind of nitride red fluorescent powder and preparation method thereof
CN111100634A (en) * 2019-12-25 2020-05-05 武汉工程大学 Long-afterglow fluorescent material and preparation method thereof

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Application publication date: 20130327