CN103351861A - Tm and Eu mono/co-doped lutecium gallium garnet phosphor - Google Patents
Tm and Eu mono/co-doped lutecium gallium garnet phosphor Download PDFInfo
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- CN103351861A CN103351861A CN2012100968259A CN201210096825A CN103351861A CN 103351861 A CN103351861 A CN 103351861A CN 2012100968259 A CN2012100968259 A CN 2012100968259A CN 201210096825 A CN201210096825 A CN 201210096825A CN 103351861 A CN103351861 A CN 103351861A
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Abstract
The invention provides a Tm and Eu mono/co-doped lutecium gallium garnet phosphor. The chemical formula of the phosphor is Lu(3-x-y)Ga5O12:xEu<3+>, yTm<3+>, wherein x is 0-0.04, y is 0-0.02, and x and y cannot be zero simultaneously. Uniform ion mixing is realized through a low temperature combustion method, and the prepared phosphor has the characteristics of spumous and loose structure, no clustering, easy ball milling and high purity. The method has the characteristics of substantial reduction of the furnace temperature, and simple production process, and is an efficient energy-saving synthesis method. The obtained phosphor has a narrow emission peak, has a peak width at half height of 4-5nm, and emits different-color light under the excitation of 241nm light, red light is emitted when only Eu<3+> is doped, blue light is emitted when only Tm<3+> is doped, white light is emitted when Eu<3+> and Tm<3+> are codoped, the phosphor can be compounded with an ultraviolet LED chip to realize white light emission.
Description
Technical field
The invention belongs to the luminescent material technical field, particularly the thulium used of a kind of white light emitting diode, europium list/mix altogether lutetium Ga garnet (LGG) fluorescent material.
Background technology
White light LEDs has less energy consumption, the advantage such as pollution-free, be called the 4th generation lighting source, have broad application prospects
[1]At present, the method for realization white light LEDs mainly contains three kinds
[2]: the one, fluorescent material light transformation approach, the blue-light excited YAG:Ce that launches with GaN base chip
3+Fluorescent material, the two light that sends of chip and fluorescent material mixes the formation white light; The 2nd, the multi-chip method, the led chip with three kinds of colors of RGB utilizes three primary color theory, sends white light according to certain ratio combination; The 3rd, integrated single-chip method (also being the Multiple Quantum Well method), Multiple Quantum Well method are to utilize a plurality of active coatings to make led chip directly send white light in a chip.The factors such as balance technology, technique, production cost, light conversion hysteria white light LEDs are one, and over-all properties is moderate, cost is lower, may realize at no distant date the approach and means of industrialization.The method is that it also is the most ripe using at most at present.It can satisfy white light LEDs as general illumination requirements such as pilot lamp, signal lamps, but shortcoming is also fairly obvious, owing to be the white light that gold-tinted and blue light two primary colours are compounded to form, has lacked red composition, so colour rendering index is on the low side
[3]LED need to have the purity height with red fluorescence powder, stable chemical nature, the high requirement of emissive porwer.Although people widely study three primary colors fluorescent powder, up to the present, people also do not obtain well-content three primary colors fluorescent powder material, especially are applied to the red fluorescence material of white light LEDs.Therefore, become indoor solid-state illumination light source of new generation if white light LEDs will replace luminescent lamp, then need to have higher luminous efficiency, higher color developing and the colour temperature of white light emission have better adjustability etc.
[4]
The lutetium Ga garnet is called for short LGG (Lutetium Gallium Garnet), and chemical formula is Lu
3Ga
5O
12, have good physics and chemistry stability, high emissive porwer, quantum yield and stable chromaticity coordinates, optical isotropy, the free of birefringence effect, the advantages such as anti-high-level radiation and electronics bombardment are widely used as the matrix of luminescent material.At present, the lutetium Ga garnet mainly is to be prepared into bulky crystal and to be applied to the laser apparatus aspect, and the correlative study of the lutetium Ga garnet powder that it is rare earth ion doped is very few
[5,6]The garnet structure material mainly adopts the preparation of conventional high-temperature solid phase method
[7,8]The product crystal grain of the method preparation is thicker, needs block sinter ball milling during application, and this process can be destroyed the crystalline form of luminescent material, and affects its luminous intensity.In recent years, liquid-phase coprecipitation successfully is used for the preparation of rear-earth-doped garnet structure fluorescent material
[9,10]Liquid-phase coprecipitation namely adds precipitation agent in the Ar ion mixing liquid on the sunny side, obtains the rear-earth-doped garnet phosphor powder body of polycrystalline after gained precursor precipitate drying, the calcining.But also there are some shortcomings in these products of coprecipitation method preparation: 1. because the difference of solubility product, subsidence rate is difficult to form pioneer's powder of precise chemical structure metering ratio, component homogeneous; 2. being difficult to control suitable pH value precipitates the positively charged ion in the mixed solution simultaneously fully; 3. the precursor powder of gained may be reunited in washing and drying process.
Summary of the invention
In order to solve the problem of prior art, it is even to the invention provides size distribution, and high thulium, the europium list/mix altogether lutetium Ga garnet fluorescent material of product purity of color, and ought singly mix respectively Eu
3+, Tm
3+And Eu
3+And Tm
3+When mixing altogether, under the exciting of 241nm light, send the light of different colours, singly mix Eu
3+The time send out light orange red, singly mix Tm
3+The time blue light-emitting, Eu
3+And Tm
3+Rubescent when mixing altogether-blue mixed light, and final and the compound realization white light emission of ultraviolet LED chip.
The present invention is achieved by the following technical solutions:
A kind of thulium of the present invention, europium list/mix altogether lutetium Ga garnet (LGG) fluorescent material, its chemical formula is Lu
(3-x-y)Ga
5O
12: xEu
3+, yTm
3+, x=0～0.04 wherein, y=0～0.02, x, y are not zero simultaneously;
Described a kind of thulium, europium list/mix altogether the preparation method of lutetium Ga garnet (LGG) fluorescent material, it may further comprise the steps:
1) by proportioning, with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Europium nitrate, thulium nitrate, lutecium nitrate are dissolved in deionized water; Two kinds of solution are mixed, be made into metal ion solution; Described Eu
3+: Tm
3+: Lu
3+: Ga
3+Mol ratio be x: y: (3-x-y): 5, x=0～0.04 wherein, y=0～0.02, x, y are not zero simultaneously;
2) in step 1) add citric acid by proportioning in the metal ion solution for preparing, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) with step 2) mixing solutions of gained is placed in the water-bath in 80 ℃ of constant temperature 0.5～1h, until all become light yellow gel;
4) with step 3) gel of gained moves in the baking oven, and in 250 ℃ of constant temperature 2～4h, gel combustion obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 800～1100 ℃, and constant temperature 2h then obtains thulium, europium list/mix altogether lutetium Ga garnet (LGG) fluorescent material.
Beneficial effect: a kind of thulium provided by the invention, europium list/mix altogether lutetium Ga garnet (LGG) fluorescent material, its chemical formula is Lu
(3-x-y)Ga
5O
12: xEu
3+, yTm
3+, x=0～0.04 wherein, y=0～0.02, x, y are not zero simultaneously; It is high to utilize low-temperature combustion method to realize that even mixing on the ion concentration, prepared product present spumescence, loose, not conglomeration, easily ball milling, and product purity of color.The furnace temperature of the method reduces greatly, and production process is easy, is a kind of energy-efficient synthetic method.Resulting fluorescent material emission peak is narrow, and peak width at half height only is 4～5nm, and, under the exciting of 241nm light, send the light of different colours, singly mix Eu
3+The time send out light orange red, singly mix Tm
3+The time blue light-emitting, Eu
3+And Tm
3+Emit white light when mixing altogether, and final and the compound realization white light emission of ultraviolet LED chip.
Description of drawings
Fig. 1 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+The XRD figure spectrum of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 2 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+The scanning electron microscope (SEM) photograph of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 3 is Lu of the present invention
2.98Ga
5O
12: 0.02Tm
3+The scanning electron microscope (SEM) photograph of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 4 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+The particle diameter Nogata distribution plan of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 5 is Lu of the present invention
2.98Ga
5O
12: 0.02Tm
3+The particle diameter Nogata distribution plan of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 6 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+The excitation-emission spectrum of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 7 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+The excitation-emission spectrum of singly mixing lutetium Ga garnet (LGG) fluorescent material.
Fig. 8 is Lu of the present invention
2.96Ga
5O
12: 0.02Tm
3+The excitation-emission spectrum of mixing altogether lutetium Ga garnet (LGG) fluorescent material.
Fig. 9 is Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+, Lu
2.98Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+And Lu
2.96Ga
5O
12: 0.02Tm
3+The CIE chromaticity coordinates of lutetium Ga garnet (LGG) fluorescent material.
Embodiment
Below by embodiment the present invention is elaborated.
1 one kinds of europium lists of embodiment are mixed lutetium Ga garnet (LGG) fluorescent material, and chemical formula is Lu
2.98Ga
5O
12: 0.02Eu
3+
1) with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Europium nitrate and lutecium nitrate are dissolved in deionized water, two kinds of solution are mixed, be made into metal ion solution; Wherein, Lu
3+: Eu
3+: Ga
3+Mol ratio is 2.98: 0.02: 5;
2) add citric acid in the metal ion mixed solution for preparing to step 1, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) mixing solutions with step 2 is placed in the water-bath in 80 ℃ of constant temperature 0.5h, until all become light yellow gel;
4) light yellow gel with step 3 moves in the baking oven, in 250 ℃ of constant temperature 2h, obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 1000 ℃, and constant temperature 2h, makes the europium list and mixes lutetium Ga garnet fluorescent material, and chemical formula is Lu
2.98Ga
5O
12: 0.02Eu
3+
The chemical formula that makes is Lu
2.98Ga
5O
12: 0.02Eu
3+The europium list is mixed lutetium Ga garnet fluorescent material particle diameter and is evenly distributed, and mean sizes is 100nm, can effectively be excited by the 241nm UV-light, realizes strong red emission, and 594nm place emission peak is very narrow, and peak width at half height (FWHM) only is 4nm, therefore has purer colourity.
2 one kinds of europium lists of embodiment are mixed lutetium Ga garnet (LGG) fluorescent material, and its chemical formula is Lu
2.96Ga
5O
12: 0.04Eu
3+
1) with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Europium nitrate and lutecium nitrate are dissolved in deionized water, two kinds of solution are mixed, be made into metal ion solution; Wherein, Lu
3+: Eu
3+: Ga
3+Mol ratio is 2.96: 0.04: 5;
2) add citric acid in the metal ion mixed solution for preparing to step 1, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) mixing solutions with step 2 is placed in the water-bath in 80 ℃ of constant temperature 1h, until all become light yellow gel;
4) light yellow gel with step 3 moves in the baking oven, in 250 ℃ of constant temperature 4h, obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 800 ℃, and constant temperature 2h, makes the europium list and mixes lutetium Ga garnet fluorescent material, and chemical formula is Lu
2.96Ga
5O
12: 0.04Eu
3+
3 one kinds of europium lists of embodiment are mixed lutetium Ga garnet (LGG) fluorescent material, and its chemical formula is Lu
2.99Ga
5O
12: 0.01Eu
3+
1) with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Europium nitrate and lutecium nitrate are dissolved in deionized water, two kinds of solution are mixed, be made into metal ion solution; Wherein, Lu
3+: Eu
3+: Ga
3+Mol ratio is 2.99: 0.01: 5;
2) add citric acid in the metal ion mixed solution for preparing to step 1, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) mixing solutions with step 2 is placed in the water-bath in 80 ℃ of constant temperature 0.8h, until all become light yellow gel;
4) light yellow gel with step 3 moves in the baking oven, in 250 ℃ of constant temperature 2h, obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 1100 ℃, and constant temperature 2h, makes the europium list and mixes lutetium Ga garnet fluorescent material, and chemical formula is Lu
2.99Ga
5O
12: 0.01Eu
3+
4 one kinds of thulium lists of embodiment are mixed lutetium Ga garnet (LGG) fluorescent material, and its chemical formula is Lu
2.98Ga
5O
12: 0.02Tm
3+
1) with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Thulium nitrate and lutecium nitrate are dissolved in deionized water, two kinds of solution are mixed, be made into metal ion solution; Wherein, Lu
3+: Tm
3+: Ga
3+Mol ratio is 2.98: 0.02: 5;
2) add citric acid in the metal ion mixed solution for preparing to step 1, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) mixing solutions with step 2 is placed in the water-bath in 80 ℃ of constant temperature 0.5h, until all become light yellow gel;
4) light yellow gel with step 3 moves in the baking oven, in 250 ℃ of constant temperature 2h, obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 1000 ℃, and constant temperature 2h, makes the thulium list and mixes lutetium Ga garnet fluorescent material, and chemical formula is Lu
2.98Ga
5O
12: 0.02Tm
3+
Prepared chemical formula is Lu
2.98Ga
5O
12: 0.02Tm
3+The thulium list is mixed lutetium Ga garnet fluorescent material and is possessed the uniform characteristics of size distribution, can effectively be excited by the 241nm UV-light, realizes strong blue emission, and the emission peak at 479nm place is very narrow, and peak width at half height (FWHM) only is 5nm.
5 one kinds of thulium lists of embodiment are mixed lutetium Ga garnet (LGG) fluorescent material, and its chemical formula is Lu
2.99Ga
5O
12: 0.01Tm
3+Described preparation method's step and condition are with embodiment 4.
6 one kinds of thuliums of embodiment, europium are mixed lutetium Ga garnet (LGG) fluorescent material altogether, and its chemical formula is Lu
2.96Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+
1) with the concentrated nitric acid dissolving of gallium oxide powder with massfraction 69%; Thulium nitrate and europium nitrate, lutecium nitrate are dissolved in deionized water, two kinds of solution are mixed, be made into metal ion solution; Wherein, Lu
3+: Eu
3+: Tm
3+: Ga
3+Mol ratio is 2.96: 0.02: 0.02: 5;
2) add citric acid in the metal ion mixed solution for preparing to step 1, mix to get mixing solutions, wherein the mol ratio of citric acid and all metal ions content sum is 1.5: 1;
3) mixing solutions with step 2 is placed in the water-bath in 80 ℃ of constant temperature 0.5h, until all become light yellow gel;
4) light yellow gel with step 3 moves in the baking oven, in 250 ℃ of constant temperature 2h, obtains the bulk powder of chocolate;
5) with step 4) the bulk powder of chocolate temperature rise rate with 2 ℃/min in the temperature programming stove of gained rises to 1000 ℃, and constant temperature 2h, makes thulium, europium and mixes altogether lutetium Ga garnet fluorescent material, and chemical formula is Lu
2.96Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+
Prepared chemical formula is Lu
2.96Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+Thulium, europium are mixed lutetium Ga garnet fluorescent material altogether, can effectively be excited by the 241nm UV-light, realize white light emission.
7 one kinds of thuliums of embodiment, europium are mixed lutetium Ga garnet (LGG) fluorescent material altogether, and chemical formula is Lu
2.94Ga
5O
12: 0.04Eu
3+, 0.02Tm
3+Described preparation method's step 3 is placed in the water-bath mixing solutions of step 2 in 80 ℃ of constant temperature 1h, until all become light yellow gel; Remaining is with embodiment 6.
8 one kinds of thuliums of embodiment, europium are mixed lutetium Ga garnet (LGG) fluorescent material altogether, and its chemical formula is Lu
2.98Ga
5O
12: 0.01Eu
3+, 0.01Tm
3+Described preparation method is with embodiment 6.
As shown in Figure 1, Lu
2.98Ga
5O
12: 0.02Eu
3+singly mix lutetium Ga garnet (LGG) fluorescent material, can successfully be made at 800～1100 ℃ of constant temperature 2h, and can with Lu
3Ga
5O
12XRD spectra corresponding, relatively find in the product degree of crystallinity of 1000 ℃ of gained best.
By Fig. 2-5 as can be known, Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+, Lu
2.98Ga
5O
12: 0.02Tm
3+Lutetium Ga garnet (LGG) the fluorescent material particle diameter of singly mixing be evenly distributed, mean sizes is 100nm.
By Fig. 6,7,8 as can be known, Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+, Lu
2.98Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+And Lu
2.96Ga
5O
12: 0.02Tm
3+Lutetium Ga garnet (LGG) fluorescent material can effectively be excited by the 241nm UV-light, obtains respectively strong ruddiness, red-blue mixed light and blue light.
As shown in Figure 9, Lu of the present invention
2.98Ga
5O
12: 0.02Eu
3+, Lu
2.98Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+And Lu
2.96Ga
5O
12: 0.02Tm
3+Lutetium Ga garnet (LGG) fluorescent material is under the 241nm ultraviolet excitation, and the CIE coordinate of gained lays respectively at (0.558,0.432), and (0.338,0.326) and (0.136,0.133) namely sends respectively ruddiness, white light and blue light.
Reference:
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[3] Yang Xiaowei translates. the development [J] of high brightness, pure white LED lamp. and Chinese electric lighting, 2000,1:27-29
[4]J.K.Park，M.A.Lim，C.H.Kim，et?al.White?light-emitting?diodes?of?GaN-based?Sr
2SiO
4:Eu?and?the?luminescent?properties，Applied?Physics?Letters，2003，82(5)，683-685.
[5]Xuesheng?Chen，Baldassare?Di?Bartolo，Norman?P.?Barnes，et?al.Thermal?tuning?and?broadening?of?the?spectral?lines?of?trivalent?neodymium?in?laser?crystals[J].phys.stat.sol.(b)，2004，8：1957-1976.
[6]Kei?Kamada，Takayuki?Yanagida，Jan?Pejchal，et?al.?Composition?engineering?in?Ce?doped?(Lu，Gd)
3(Ga，Al)
5O
12single?crystal?scintillators[J].Cryst.Growth?Des.，2011，11(10)：pp?4484-4490.
[7]Jia，W.；Liu，H.；Wang，Y.；Hommerich，U.；Eilers，H.；Hoffman，K.R.；Yen，W.M.Origin?of?the?NIR?emission?in?Cr-doped?forsterite，Y
3Al
5O
12and?Y
2SiO
5[J].J.Lumin.，1994，60：158-162.
[8]Zhongfei?Mu，Yihua?Hu，Haoyi?Wu，et?al.Luminescence?and?energy?transfer?of?Mn
2+and?Tb
3+?in?Y
3Al
5O
12phosphors.Journal?ofAlloys?and?Compounds.201l，509(22)：6476-6480.
[9] Li Xueming, Tao Chuanyi, Kong Lingfeng, etc. submicron order Y
3A
15O
12: Ce
3+The coprecipitation method of fluorescent material is synthetic, sign and photoluminescence [J]. Chinese Journal of Inorganic Chemistry, 2007,8:1409-1414.
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Claims (9)
1. a thulium, europium list/mix altogether lutetium Ga garnet fluorescent material is characterized in that its chemical formula is Lu
(3-x-y)Ga
5O
12: xEu
3+, yTm
3+, x=0～0.04 wherein, y=0～0.02, x, y are not zero simultaneously.
2. a fluorescent material according to claim 1 is characterized in that, it mixes lutetium Ga garnet fluorescent material for the europium list, it is characterized in that, its chemical formula is Lu
2.98Ga
5O
12: 0.02Eu
3+
3. a fluorescent material according to claim 1 is characterized in that, it mixes lutetium Ga garnet fluorescent material for the europium list, and its chemical formula is Lu
2.96Ga
5O
12: 0.04Eu
3+
4. a fluorescent material according to claim 1 is characterized in that, it mixes lutetium Ga garnet fluorescent material for the europium list, and its chemical formula is Lu
2.99Ga
5O
12: 0.01Eu
3+
5. a fluorescent material according to claim 1 is characterized in that, it mixes lutetium Ga garnet fluorescent material for the thulium list, and its chemical formula is Lu
2.98Ga
5O
12: 0.02Tm
3+
6. a fluorescent material according to claim 1 is characterized in that, it mixes lutetium Ga garnet fluorescent material for the thulium list, and its chemical formula is Lu
2.99Ga
5O
12: 0.01Tm
3+
7. a fluorescent material according to claim 1 is characterized in that, it is that thulium, europium are mixed lutetium Ga garnet fluorescent material altogether, and its chemical formula is Lu
2.96Ga
5O
12: 0.02Eu
3+, 0.02Tm
3+
8. a fluorescent material according to claim 1 is characterized in that, it is that thulium, europium are mixed lutetium Ga garnet fluorescent material altogether, and its chemical formula is Lu
2.94Ga
5O
12: 0.04Eu
3+, 0.02Tm
3+
9. a fluorescent material according to claim 1 is characterized in that, it is that thulium, europium are mixed lutetium Ga garnet fluorescent material altogether, and its chemical formula is Lu
2.98Ga
5O
12: 0.01Eu
3+, 0.01Tm
3+
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| JP2012041538A (en) * | 2011-09-20 | 2012-03-01 | Fujifilm Corp | Inorganic compound and composition and molded body containing the same, light-emitting device, and solid laser device |
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2012
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