CN103571461A - Rare earth silicate blue-yellow fluorescent material for high-color-rendering energy saving lamp and preparation method - Google Patents

Rare earth silicate blue-yellow fluorescent material for high-color-rendering energy saving lamp and preparation method Download PDF

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Publication number
CN103571461A
CN103571461A CN201310539737.6A CN201310539737A CN103571461A CN 103571461 A CN103571461 A CN 103571461A CN 201310539737 A CN201310539737 A CN 201310539737A CN 103571461 A CN103571461 A CN 103571461A
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China
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fluorescent material
rare earth
saving lamp
earth silicate
preparation
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陈小英
周建明
张建明
姜发祥
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QUZHHOU OST LIGHTING Co Ltd
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QUZHHOU OST LIGHTING Co Ltd
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Abstract

The invention relates to a rare earth silicate blue-yellow fluorescent material for a high-color-rendering energy saving lamp and a preparation method, aiming to obtain a rare earth fluorescent material for the energy saving lamp with high color rendering index by adopting the method and material provided by the invention. The general formula of the rare earth silicate blue-yellow fluorescent material for the high-color-rendering energy saving lamp is M<2x-a>Mg<y>Si2O7:aRe, wherein M is one or a composition of more than one of Ca, Sr and Ba; Re is one or a composition of more than one of Ce, Eu, Dy, Ho, Er, Tm and Yb; x is equal to 0.8-1; y is equal to 0.8-1; a is equal to 0-0.3. The preparation method comprises the following steps: weighing all the components in the raw materials according to the stoichiometric ratio in the general formula M<2x-a>Mg<y>Si2O7:aRe, grinding the components and mixing the powder uniformly, then putting the mixture in a crucible and carrying out firing once or multiple times in a high temperature furnace at 800-1400 DEG C under the reducing atmosphere, thus obtaining the rare earth silicate blue-yellow fluorescent material for the high-color-rendering energy saving lamp.

Description

Used for high-color developing energy-saving lamp rare earth silicate indigo plant, gold-tinted fluorescent material and preparation method
Technical field
The present invention relates to a class silicate luminescent material, it can be inspired blue-yellow light effectively in 250-410nm scope; It is mixed with rare earth luminescent material with trichromatic energy saving lamp, can obtain used for high color rendering property energy-saving lamp rare-earth luminescent material.
Background technology
In conventional lighting, rare-earth trichromatic energy saving lamp still occupies sizable ratio; Colour rendering index is an important indicator weighing electricity-saving lamp performance, rare-earth trichromatic fluorescent material (rouge and powder (Y 2o 3: Eu 3+), green powder (CeTbMgAl 11o 19), blue powder (BaMgAl 10o 17: Eu 2+) narrow-band spectrum, the discontinuity of the emmission spectrum of this electricity-saving lamp determined the colour temperature made with it at the colour rendering index of 2300-8000K electricity-saving lamp generally in 80 left and right; Therefore, only make up the deficiency of three primary colours line spectrum wave band, could improve into the colour rendering index after lamp.
Research shows: increase emmission spectrum at 430～490nm, the emmission spectrum of 520～565nm can improve the colour rendering index of electricity-saving lamp.Therefore, seek suitable fluorescent material and make up electricity-saving lamp at 430～490nm, the emmission spectrum of 520～565nm becomes study hotspot all the time.
The research of silicate fluorescent material relatively early, is a class fluor that obtains the earliest application, as Mn 2+the zinc silicate and the beryllium zinc silicate that activate are the green-emitting phosphors that is used as the earliest luminescent lamp and CRT monitor.Alkaline-earth silicate is the efficient substrate material of supporting rare earth luminescence, has good stability, and the feature such as emmission spectrum wide coverage, is also the focus system of the fluorescent material research of various ranges of application always.
Summary of the invention
The object of this invention is to provide a kind of silicate fluorescent material and corresponding preparation method, institute's fluorescent material that obtains should the effective excitation-emission of quilt go out indigo plant, green glow under the incident beam of 250-410nm, by itself and rare-earth trichromatic fluorescent material rouge and powder (Y 2o 3: Eu 3+), green powder (CeTbMgAl 11o 19), blue powder (BaMgAl 10o 17: Eu 2+) after fluorescent material mixes, can obtain the electricity-saving lamp rare-earth luminescent material that colour rendering index is high.
Technical scheme provided by the invention is: used for high-color developing energy-saving lamp rare earth silicate is blue, gold-tinted fluorescent material, and the general formula that it is characterized in that this fluorescent material is M 2x-amg ysi 2o 7: aRe; Wherein: M is one or more the combination in Ca, Sr, Ba, Re is one or more the combination in Ce, Eu, Dy, Ho, Er, Tm or Yb, x=0.8-1; Y=0.8-1; A=0-0.3.
In this fluorescent material, is also furnished with the boric acid of thousandth to thousand/ten mass ratio.
Used for high-color developing energy-saving lamp rare earth silicate is blue, the preparation method of gold-tinted fluorescent material, and step is: by all the components in raw material according to formula M 2xmg ysi 2o 7: the metering ratio of aRe weighs up, and after being ground, puts into crucible, and in High Temperature Furnaces Heating Apparatus 800-1400 ℃ temperature range, under reducing atmosphere, through one or many, calcination obtains.
Described calcination time is 1-6 hour.
Described reducing atmosphere is hydrogen-nitrogen mixture gas, and density of hydrogen is 1-12%.
The granularity of described fluorescent material is 5-10um.
Described rare earth silicate is blue, gold-tinted fluorescent material, and its precursor raw material also can be prepared by sol-gel method or the precipitator method, can be also oxide compound or salt, then obtain by high temperature solid state reaction.
The invention has the beneficial effects as follows: silicate fluorescent material provided by the invention, can be by adjusting M ion and Eu 2+ratio, obtain having at about 440nm to 550nm place the multiple fluorescent material of peak value, and the launching efficiency at ultraviolet region 250-410nm is also higher, can effectively absorbs the mercury line of 254 in electricity-saving lamp, 365,403nm, and then can improve the colour rendering index of electricity-saving lamp.It is mixed by different ratios with rare-earth trichromatic fluorescent material, just can obtain the rare-earth luminescent material for electricity-saving lamp (colour rendering index is increased to more than 90 from original 80) of high-color rendering.And this class fluorescent material is all to take silicate substrate as host lattice, and material has consistent stability, thereby the electricity-saving lamp obtaining also has satisfactory stability and consistence.
Accompanying drawing explanation
The fluorescent material Ca of Yellow light-emitting low temperature in Fig. 1 the present invention 1.97mgSi 2o 7: aEu 2+(a=0.03) excitation spectrum under room temperature and emmission spectrum.
Fig. 2 is the fluorescent material Sr of blue light-emitting in the present invention 1.97mgSi 2o 7: aEu 2+(a=0.03) excitation spectrum under room temperature and emmission spectrum.
Embodiment
Fluorescent material in the present invention obtains by high temperature solid state reaction; Concrete grammar is using the oxide compound of the M as raw material or carbonate, silicon-dioxide, rare earth oxide, and as a small amount of boric acid (thousandth to thousand of total mass/ten) of fusing assistant, the stoichiometric ratio definite according to general formula weighs up, and after being ground, puts into corundum crucible, in High Temperature Furnaces Heating Apparatus 800-1400 ℃ temperature range (preferably 1200-1400 ℃), reducing atmosphere (reducing atmosphere is hydrogen-nitrogen mixture gas, density of hydrogen 1-12%) is lower to be obtained through calcination, calcination time 3-6 hour.After the fluorescent material ball mill pulverizing obtaining by aforesaid method, (5-10um) obtains fluorescent material used in the present invention.
In Fig. 1 and Fig. 2, can find out: the fluorescent material obtaining as stated above effectively exciting within the scope of 250-410nm is very clear, they can be by the optical excitation of this wavelength region, launch indigo plant, green glow, so this fluorescent material is applicable to make up the spectrum of trichromatic energy saving lamp.
Below in conjunction with embodiment, further explain the preparation of high colour developing Energy-Saving Lamps fluorescent material in the present invention, the following examples only, for explanation, should not form the restriction to the scope of protection of present invention.
Powder process embodiment 1
Ca 1.97mgSi 2o 7: Eu 0.03preparation: take raw material
CaCO 3:3.9401g
MgO:0.8062g
SiO 2:2.4032g
Eu 2O 3:0.1056g
H 3BO 3:0.0429g
After above-mentioned raw materials is ground and mixed, in 1000 ± 20 ℃ of temperature ranges of High Temperature Furnaces Heating Apparatus, under reducing atmosphere, (hydrogen-nitrogen mixture gas, density of hydrogen 4-8%) obtains through the calcination of 4 hours.After fluorescent material ball mill pulverizing to the 6 ± 1um obtaining by aforesaid method, obtain fluorescent material used in the present invention; Its excitation spectrum 1 and emmission spectrum 2 are as shown in Figure 1.
Powder process embodiment 2
Sr 1.97mgSi 2o 7: Eu 0.03preparation: take raw material
SrCO 3:5.8166g
MgO:0.8062g
SiO 2:2.4032g
Eu 2O 3:0.1056g
H 3BO 3:0.0542g
After above-mentioned raw materials is ground and is mixed, in 1200 ± 20 ℃ of temperature ranges of High Temperature Furnaces Heating Apparatus, (hydrogen-nitrogen mixture gas under reducing atmosphere, density of hydrogen 6-10%) through twice calcination, obtain, calcination for the first time 3 hours, room temperature is after cooling 1 hour, calcination for the second time 2 hours.The fluorescent material ball mill pulverizing obtaining by aforesaid method obtains fluorescent material used in the present invention to 8um; The excitation spectrum 1 and the emmission spectrum 2 that in Fig. 2, have shown this material.
Lamp embodiment 1 processed
The fluorescent material that above method makes mixes by following mass ratio with trichromatic rare-earth luminescent material: Sr 1.97mgSi 2o 7: Eu 0.03(5-25%), Ca 1.97mgSi 2o 7: Eu 0.03(5-20%), rouge and powder Y 2o 3: Eu 3+(20-30%), green powder CeTbMgAl 11o 19(15-35%), blue powder BaMgAl 10o 17: Eu 2+(10-25%) can make more than 88 electricity-saving lamp of colour rendering index.
Tricolor powder arranges in pairs or groups that silicate of the present invention is blue, gold-tinted fluorescent material kind ratio and lamp parameter processed be as following table:
Tricolor powder and powder of the present invention collocation Light efficiency Coordinate Colour temperature Aobvious finger Powder kind ratio
YOX:CAT:BAM 70.2 0.3136/0.3439 6583K 81.2 41:36:23
YOX:CAT:BAM：Sr（Ca）MgSi 2O 7:Eu 68.3 0.3133/0.3443 6552K 98.3 40:32：21:7
YOX:CAT:BAM：Sr（Ca）MgSi 2O 7:Eu 68.0 0.3138/0.3449 6543K 98.6 41:31：19:9
YOX:CAT:BAM：Sr（Ca）MgSi 2O 7:Eu 67.5 0.3133/0.3443 6532K 88.8 42:31：16:11
In table: YOX is rouge and powder, CAT is green powder, and BAM is blue powder;
Sr(Ca) MgSi 2o 7: Eu is the present invention (Sr 1.97mgSi 2o 7: Eu 0.03with Ca 1.97mgSi 2o 7: Eu 0.03be 1: 1 proportioning).

Claims (7)

1. blue, the gold-tinted fluorescent material of used for high-color developing energy-saving lamp rare earth silicate, the general formula that it is characterized in that this fluorescent material is M 2x-amg ysi 2o 7: aRe; Wherein: M is one or more the combination in Ca, Sr, Ba, Re is one or more the combination in Ce, Eu, Dy, Ho, Er, Tm or Yb, x=0.8-1; Y=0.8-1; A=0-0.3.
2. used for high-color developing energy-saving lamp rare earth silicate indigo plant according to claim 1, gold-tinted fluorescent material, is characterized in that: the boric acid of being also furnished with thousandth to thousand/ten mass ratio in this fluorescent material.
3. the preparation method of blue, the gold-tinted fluorescent material of used for high-color developing energy-saving lamp rare earth silicate, step is: by all the components in raw material according to formula M 2xmg ysi 2o 7: the metering ratio of aRe weighs up, and after being ground, puts into crucible, and in High Temperature Furnaces Heating Apparatus 800-1400 ℃ temperature range, under reducing atmosphere, through one or many, calcination obtains.
4. the preparation method of used for high-color developing energy-saving lamp rare earth silicate indigo plant according to claim 3, gold-tinted fluorescent material, is characterized in that: described calcination time is 1-6 hour.
5. the preparation method of used for high-color developing energy-saving lamp rare earth silicate indigo plant according to claim 4, gold-tinted fluorescent material, is characterized in that: described reducing atmosphere is hydrogen-nitrogen mixture gas, and density of hydrogen is 1-12%.
6. the preparation method of used for high-color developing energy-saving lamp rare earth silicate indigo plant according to claim 5, gold-tinted fluorescent material, is characterized in that: the granularity of described fluorescent material is 5-10um.
7. the preparation method of blue, the gold-tinted fluorescent material of used for high-color developing energy-saving lamp rare earth silicate according to claim 6, it is characterized in that: described rare earth silicate is blue, gold-tinted fluorescent material, its precursor raw material also can be prepared by sol-gel method or the precipitator method, also can be oxide compound or salt, then obtain by high temperature solid state reaction.
CN201310539737.6A 2013-11-04 2013-11-04 Rare earth silicate blue-yellow fluorescent material for high-color-rendering energy saving lamp and preparation method Pending CN103571461A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1948426A (en) * 2006-11-08 2007-04-18 天津大学 Preparation method of nanometer silicate long afterglow luminous material
US20090058255A1 (en) * 2007-08-31 2009-03-05 Hitoshi Oaku Plasma display device
CN102533259A (en) * 2011-10-25 2012-07-04 重庆文理学院 Silicate green fluorescent powder for white light emitting diode (LED) and preparation method for fluorescent powder
CN103087709A (en) * 2013-01-24 2013-05-08 陕西科技大学 Cerium-ion-doped silicate blue fluorescent powder and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1948426A (en) * 2006-11-08 2007-04-18 天津大学 Preparation method of nanometer silicate long afterglow luminous material
US20090058255A1 (en) * 2007-08-31 2009-03-05 Hitoshi Oaku Plasma display device
CN102533259A (en) * 2011-10-25 2012-07-04 重庆文理学院 Silicate green fluorescent powder for white light emitting diode (LED) and preparation method for fluorescent powder
CN103087709A (en) * 2013-01-24 2013-05-08 陕西科技大学 Cerium-ion-doped silicate blue fluorescent powder and preparation method thereof

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Application publication date: 20140212