CN104250555A - Yellow fluorescent powder and preparation method thereof and light emitting device using fluorescent powder - Google Patents

Yellow fluorescent powder and preparation method thereof and light emitting device using fluorescent powder Download PDF

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Publication number
CN104250555A
CN104250555A CN201310262528.1A CN201310262528A CN104250555A CN 104250555 A CN104250555 A CN 104250555A CN 201310262528 A CN201310262528 A CN 201310262528A CN 104250555 A CN104250555 A CN 104250555A
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fluorescent powder
yellow fluorescent
fluorescent material
powder
analytical pure
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张日光
周天亮
朱小清
林胜
王义飞
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NINGBO SUNPU-OPTO SEMICONDUCTOR Co Ltd
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NINGBO SUNPU-OPTO SEMICONDUCTOR Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/4805—Shape
    • H01L2224/4809—Loop shape
    • H01L2224/48091—Arched
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/481—Disposition
    • H01L2224/48151—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
    • H01L2224/48221—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
    • H01L2224/48245—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic
    • H01L2224/48247—Connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being metallic connecting the wire to a bond pad of the item

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Abstract

The invention discloses a yellow fluorescent powder and a preparation method thereof and a light emitting device prepared from the fluorescent powder. The fluorescent powder has the chemical formula of A[x]Z[y]Ce[3-x-y]E[m]D[5-m]O[12], wherein A is one or more elements of La, Y, Lu and Tb, Z is one or more elements of Zn, Mg, Ca, Sr and Ba, E is one or more elements of Al, In and Ga, D is one or two of Si and Ge, 0<x<3, 0<y<=0.2, x+y<3, 4.8<=m<5, and y+m=5. The yellow fluorescent powder has the advantages of low production cost, simple process and higher light emitting intensity.

Description

Yellow fluorescent powder and preparation method thereof and the luminescent device using this fluorescent material
Technical field
The present invention relates to a kind of yellow fluorescent powder, the luminescent device that the preparation method that the invention still further relates to this fluorescent material makes with this fluorescent material, is phosphor technical field.
Background technology
LED (Light emitting diode) is a kind of can be the semiconducter device of luminous energy by electric energy conversion.Due to white light LEDs have efficiently, energy-saving and environmental protection, firm in structure, long service life and the advantage such as the time of response is short, be widely used in instruction, backlight and lighting field at present.Common white light LEDs many dependence fluorescent material conversion realizes white light and exports, and comparatively general mode comprises following two kinds:
1. three primary colors fluorescent powder conversion LED.UV-light (UV) LED is utilized to excite one group can effectively be excited by UV-light and send the fluorescent material of red, green, blue three kinds of colors.The feature of this white light LEDs is that the visible light part of spectrum in light source device is produced by fluorescent material completely.But, the electric light transformation efficiency of this type of white light LEDs is lower; Accurately mixed powder is more difficult; Packaged material is easily aging under UV-irradiation, and the life-span is shorter; There is the hidden danger that ultraviolet is revealed; Efficiently, ultraviolet LED chip can be sent not easily to prepare.
2. blue chip excites yellow fluorescent powder.In the white light LEDs of the type, the blue light that chip sends excites yellow fluorescent powder and obtains sodium yellow, and unabsorbed blue light and gold-tinted compound obtain white light.The white light LEDs of the type is the white light LEDs that degree of being practical is the most general, and the main component of the yellow fluorescent powder used is YAG:Ce (Y 3al 5o 12: Ce 3+).
Non-patent literature one " the colour TV flying-spot CRT yellow fluorescent powder Y that the luminosity of YAG:Ce was published as far back as 1967 3al 5o 12: Ce 3+" (A new phosphor for flying spot cathode ray tubes for color television:yellow emitting Y 3al 5o 12: Ce 3+, Applied Physics Letters, Volume11, Issue2,1967) have been reported in a literary composition.1996, Ya chemical company has applied for using YAG:Ce yellow fluorescent powder to obtain the US Patent No. 5998925 of white light in conjunction with blue chip, Ya chemical company is in US Patent No. 6069440 patent afterwards, disclose and replace Y by rare earth element parts such as Gd, Sm and Lu, or use Ga part to replace Al, the emmission spectrum of YAG:Ce can be made to change between 530-570nm." Ca and Si codoped is to Y for non-patent literature two 3al 5o 12: Ce 3+the impact of structure and luminescent properties " (Effect of the Co-substitution of Ca 2+and Si 4+on the Structure and Luminescence Properties of Y 3al 5o 12: Ce 3+, Advanced Materials Research, Vol.233-235,2011) in report the regulation and control adopting Ca and Si codoped can realize YAG:Ce emmission spectrum, but its luminous intensity obviously declines; " Si replaces Y non-patent literature three 3al 5o 12: Ce 3+the impact of temperature profile " (Influence of Si 4+substitution on the temperature-dependent characteristics of Y 3al 5o 12: Ce 3+chinese.Physics.B, Vol.20,2011) after reporting use Si replacement Al, the emmission spectrum of YAG:Ce can be made to move to blue light direction, but Si replaces separately the charge unbalance that Al can cause chemical formula, make to produce in the structure of fluorescent material and be used for the defect of balancing charge in a large number, finally make the luminous intensity of YAG:Ce obviously reduce; Non-patent literature four " Y prepared by spray pyrolysis 3al 5-2y(Mg, Si) yo 12: Ce 3+luminosity " (Luminescence Characteristics of Y 3al 5-2y(Mg, Si) yo 12: Ce 3+phosphor Prepared by Spray Pyrolysis, Journal of The Electrochemical Society, Vol.157,2010) one to the article pointed out, when Mg and Si replaces Al simultaneously, the emmission spectrum of YAG:Ce can be made to move to ruddiness direction; Non-patent literature five " Sr 2+to phosphor for white light LED YAG:Ce 3+the red research of increasing " (luminous journal, 11 phases in 2011) report Sr replacement Y, the emmission spectrum of YAG:Ce can be made to move to ruddiness direction, but Sr replaces separately the charge unbalance that Y can cause chemical formula, make to produce in the structure of fluorescent material and be used for the defect of balancing charge in a large number, finally make the luminous intensity of YAG:Ce obviously reduce.
YAG:Ce adopts a reductive firing technique usually.Namely the composition according to YAG:Ce is prepared burden, and after mixing, in High Temperature Furnaces Heating Apparatus, under reducing atmosphere, sintering forms, and can use afterwards by after the fluorescent powder crushing sintered, cleaning and classification.Above-mentioned aftertreatment technology can make the surface imperfection of YAG:Ce more, causes the luminous intensity of fluorescent material to decline.
In a word, YAG:Ce is a kind of excellent property yellow fluorescent powder, but lack green color components in the emmission spectrum of YAG:Ce, and the emmission spectrum of YAG:Ce is regulated and controled by appropriate means, make comprise more green color components when the luminous intensity of YAG:Ce reduces less, in its emmission spectrum, simultaneously by improvement of production process, improve the brightness of fluorescent material, then have further upward mobility with the light efficiency of the white light LEDs of YAG:Ce manufacture.
Summary of the invention
Technical problem to be solved by this invention provides for the above-mentioned state of the art yellow fluorescent powder that a kind of luminous intensity is high.
Another technical problem to be solved by this invention is to provide the preparation method of the high yellow fluorescent powder of a kind of luminous intensity.
Another technical problem to be solved by this invention is to provide the luminescent device that the high yellow fluorescent powder of a kind of luminous intensity is made.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of yellow fluorescent powder, is characterized in that: its chemical formula is A xz yce 3-x-ye md 5-mo 12wherein A is one or more elements in La, Y, Lu and Tb, Z is one or more elements in Zn, Mg, Ca, Sr and Ba, E is one or more elements in Al, In and Ga, D is one or both of Si and Ge, 0<x<3, x+y<3,4.8≤m<5, y+m=5.
In described chemical formula, 0<y≤0.2.
Described chemical formulation material is A by chemical constitution 3al 5o 12with Z 3al 2d 3o 12the system solid solution that both are formed.
Described chemical formulation material is Ce 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12the limit solid solution formed, wherein, Ce 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12molar ratio range be greater than 10 and be less than 300.
The median size of described chemical formulation material is 1 ~ 100 μm.
Extent of fluorescence under the exciting of any one light of described chemical formulation material in ultraviolet, visible ray and electron rays is 500 ~ 600nm.
A preparation method for yellow fluorescent powder, is characterized in that comprising the steps:
Oxide compound, carbonate or oxyhydroxide containing A, Z, E, D and Ce element is taken as raw material according to stoichiometric ratio according to chemical formula, at 1000 ~ 1600 DEG C, 2 ~ 10h is sintered after mixing, select the powder after one or more method process sintering in pulverizing, classification and acid treatment method, to adjust median size to 1 ~ 100 μm of powder, be washed with distilled water to neutrality; Reductase 12 ~ 10h at 1000 ~ 1400 DEG C, namely obtains yellow fluorescent powder afterwards.
A kind of luminescent device be made up of yellow fluorescent powder, it is characterized in that: comprise above-mentioned yellow fluorescent powder and illuminating source, described illuminating source is to send the photodiode of 300 ~ 490nm wavelength light, laser diode or organic EL luminous element, the colour temperature of luminescent device is greater than 6000K, and colour rendering index is greater than 75.
The luminescent device be made up of yellow fluorescent powder, is characterized in that: also include other fluorescent material, and the colour temperature of luminescent device is less than 4800K, and colour rendering index is greater than 85.
The luminescent device be made up of yellow fluorescent powder, other fluorescent material described in it is characterized in that are one or more in following fluorescent material: (Ca, Sr, Ba) 2si 5n 8: Eu, (Ca, Sr) AlSiN 3: Eu, β-SiAlON:Eu, (Ba, Sr) Y 2si 2al 2o 2n 5: Eu, Ca 2alSi 3o 2n 5: Eu, Ba 3si 6o 12n 2: Eu, (Ca, Sr, Ba) Si 2o 2n 2: Eu, Li 2ca 2si 2o 7: Eu, Cs 2mgSi 5o 12: Eu, (Ca, Sr, Ba) 2siO 4: Eu, (Ca, Sr, Ba) 2mgSi 2o 7: Eu, (Ca, Sr, Ba) 3mgSi 2o 8: Eu, BaSi 2o 5: Eu, Ba 2zn 3si 3o 11: Eu, (Ca, Sr, Ba) 2al 2siO 7: Eu, CaZrSi 2o 7: Eu, (Ca, Sr, Ba) Al 2o 4: Eu, Sr 4al 14o 25: Eu, Lu 3al 5o 12: Ce, Ca 3sc 2si 3o 12: Ce, SrAl 2b 2o 7: Eu, Sr 2b 2o 5: Eu, Ca 2al 3o 6f:Eu, Na 2siF 6: Mn.
Compared with prior art, the invention has the advantages that: yellow fluorescent powder rare-earth usage used obviously reduces, and can reduce cost of manufacture; This yellow fluorescent powder is sosoloid fluorescent material, and its structure overcomes the defect caused because of non-equilibrium replacement, makes the luminous intensity of this yellow fluorescent powder higher; Finally, by improving the synthesis technique of yellow fluorescent powder, its luminous intensity is further increased.
Accompanying drawing explanation
Fig. 1 is the excitation and emission spectra of comparative example 1 yellow fluorescent powder;
Fig. 2 is the X-ray diffraction spectrum of comparative example 1 yellow fluorescent powder;
Fig. 3 is the excitation and emission spectra of comparative example 2 yellow fluorescent powder;
Fig. 4 is the excitation and emission spectra of embodiment 1 yellow fluorescent powder;
Fig. 5 is the excitation and emission spectra of embodiment 2 yellow fluorescent powder;
Fig. 6 is the excitation and emission spectra of embodiment 3 yellow fluorescent powder;
Fig. 7 is the X-ray diffraction spectrum of embodiment 3 yellow fluorescent powder;
Fig. 8 is the excitation and emission spectra of embodiment 4 yellow fluorescent powder;
Fig. 9 is the excitation and emission spectra of embodiment 5 yellow fluorescent powder;
Figure 10 is the X-ray diffraction spectrum of embodiment 5 yellow fluorescent powder;
Figure 11 is the excitation and emission spectra of embodiment 6 yellow fluorescent powder;
Figure 12 is the excitation and emission spectra of embodiment 7 yellow fluorescent powder;
Figure 13 is the excitation and emission spectra of embodiment 8 yellow fluorescent powder;
Figure 14 is the excitation and emission spectra of embodiment 9 yellow fluorescent powder;
Figure 15 is the X-ray diffraction spectrum of embodiment 9 yellow fluorescent powder;
Figure 16 is embodiment 14 emitting device structure schematic diagram;
Figure 17 is the spectrogram of embodiment 14 luminescent device;
Figure 18 is embodiment 15 emitting device structure schematic diagram;
Figure 19 is the spectrogram of embodiment 15 luminescent device;
Figure 20 is the excitation and emission spectra of embodiment 21 yellow fluorescent powder.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
The chemical formula of comparative example 1 fluorescent material is Y 2.91ce 0.09al 5o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure) and Al 2o 3(analytical pure).Mol ratio is 1.455:0.09:2.5, raw mill mixing is placed in aluminum oxide (also can be zirconium white or boron nitride) container, 4 hours are sintered at the temperature of 1550 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas (also can be hydrogen, one or more in ammonia and carbon monoxide), powder after sintering is taken out from container, select to pulverize, classification also (also can select sulfuric acid with the hydrochloric acid that volumetric molar concentration is 3 moles often liter, nitric acid, phosphoric acid, hydrofluoric acid and organic acid pure substance or mixture) process, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1400 DEG C, reducing atmosphere is that hydrogen (also can be hydrogen nitrogen mixture, one or more in ammonia and carbon monoxide), required fluorescent material can be obtained.Fig. 1 is the excitation and emission spectra of obtained yellow fluorescent powder; Fig. 2 is the X-ray diffraction spectrum of yellow fluorescent powder.
The chemical formula of comparative example 2 fluorescent material is Y 2.89ce 0.09sr 0.02al 4.98si 0.02o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.445:0.09:0.02:2.49:0.02, raw mill mixing is placed in alumina container, 4 hours are sintered at the temperature of 1550 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, the HCl treatment that selection is pulverized, classification is also 3 moles often liter by volumetric molar concentration, can obtain required fluorescent material.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 144.5, Fig. 3 is comparative example 2 yellow fluorescent powder.
The chemical formula of embodiment 1 fluorescent material is Y 2.9ce 0.09sr 0.01al 4.99si 0.01o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.45:0.09:0.01:2.495:0.01, raw mill mixing is placed in alumina container, 4 hours are sintered at the temperature of 1550 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1400 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 290, Fig. 4 is the yellow fluorescent powder obtained.
The chemical formula of embodiment 2 fluorescent material is Y 2.89ce 0.09sr 0.02al 4.98si 0.02o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.445:0.09:0.02:2.49:0.02, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1550 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 144.5, Fig. 5 is yellow fluorescent powder.Can be found out by this figure, when chemical composition is identical with comparative example 2, by the technique of secondary reduction, the luminous intensity of fluorescent material is significantly improved.
The chemical formula of embodiment 3 fluorescent material is Y 2.88ce 0.09sr 0.03al 4.97si 0.03o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.44:0.09:0.03:2.485:0.03, raw mill mixing is placed in alumina container, 4 hours are sintered at the temperature of 1500 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1400 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 96, Fig. 6 is the yellow fluorescent powder obtained; Fig. 7 is the X-ray diffraction spectrum of yellow fluorescent powder.
The chemical formula of embodiment 4 fluorescent material is Y 2.86ce 0.09sr 0.05al 4.95si 0.05o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.43:0.09:0.05:2.475:0.05, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1490 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1400 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 57.2, Fig. 8 is the yellow fluorescent powder obtained.
The chemical formula of embodiment 5 fluorescent material is Y 2.84ce 0.09sr 0.07al 4.93si 0.07o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.42:0.09:0.07:2.465:0.07, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1480 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 41, Fig. 9 is the yellow fluorescent powder obtained; Figure 10 is the X-ray diffraction spectrum of the yellow fluorescent powder obtained.
The chemical formula of embodiment 6 fluorescent material is Y 2.82ce 0.09sr 0.09al 4.91si 0.09o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.41:0.09:0.09:2.455:0.09, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1480 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 31, Figure 11 is the yellow fluorescent powder obtained.
The chemical formula of embodiment 7 fluorescent material is Y 2.79ce 0.09sr 0.12al 4.88si 0.12o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.395:0.09:0.12:2.44:0.12, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1470 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 23, Figure 12 is the yellow fluorescent powder obtained.
The chemical formula of embodiment 8 fluorescent material is Y 2.76ce 0.09sr 0.15al 4.85si 0.15o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.38:0.09:0.15:2.425:0.15, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1460 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 18.4, Figure 13 is the yellow fluorescent powder obtained.
The chemical formula of embodiment 9 fluorescent material is Y 2.71ce 0.09sr 0.2al 4.8si 0.2o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.355:0.09:0.2:2.4:0.2, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1450 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 14, Figure 14 is the yellow fluorescent powder obtained; Figure 15 is the X-ray diffraction spectrum of yellow fluorescent powder.
The chemical formula of embodiment 10 fluorescent material is Y 2.71ce 0.09sr 0.1ba 0.1al 4.8si 0.2o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), BaCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.355:0.09:0.1:0.1:2.4:0.2, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1480 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12the mol ratio of (Ba calculates with Sr) is approximately 14.
The chemical formula of embodiment 11 fluorescent material is Y 2.46lu 0.4ce 0.09sr 0.05al 4.95si 0.05o 12
Raw material is Y 2o 3(analytical pure), Lu 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.23:0.2:0.09:0.05:2.475:0.05, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1450 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12(Lu calculates with Y) and Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately 57.2.
The chemical formula of embodiment 12 fluorescent material is Y 2.71ce 0.09sr 0.2al 4.4ga 0.4si 0.2o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure), Ga 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.355:0.09:0.2:2.2:0.2:0.2, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1500 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1380 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12the mol ratio of (Ga calculates with Al) is approximately 14.
The chemical formula of embodiment 13 fluorescent material is Y 2.61gd 0.1ce 0.09ba 0.1sr 0.1al 4.6ga 0.2si 0.2o 12
Raw material is Y 2o 3(analytical pure), Gd 2o 3(analytical pure), CeO 2(analytical pure), BaCO 3(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure), Ga 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.305:0.05:0.09:0.1:0.1:2.3:0.1:0.2, raw mill mixing is placed in zirconium white container, 4 hours are sintered at the temperature of 1450 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 20 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1350 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12(Gd calculates with Y) and Ce 3+the Sr activated 3al 2si 3o 12the mol ratio of (Ba calculates with Sr, and Ga calculates with Al) is approximately 14.
Embodiment 14
Make the white light LED luminescent device 1 shown in Figure 16.Have two lead-in wires, the groove position on the first lead-in wire 2 placed the chip 4 of blue light-emitting, and the lower electrode of chip 4 is connected with conductive resin with the bottom surface of groove, and upper electrode is connected with thin gold thread 5 with the second lead-in wire 3.
By the fluorescent material in embodiment 6 and Sr 2si 5n 8: Eu fluorescent material mixes according to the ratio of 6:1, is mixed in epoxy resin by the powder mixed with 15% mass concentration, the fluorescent material 7 mixed and epoxy resin 6 is coated on the groove position above the first lead-in wire 2 with point gum machine.Illuminating source in the present embodiment can select to send the photodiode of 300 ~ 490nm wavelength light, laser diode or organic EL luminous element.Figure 17 is the spectrogram of luminescent device, and the colour rendering index of illuminating device is 78, and colour temperature is 3008K.
Embodiment 15
Make the white light LED luminescent device 11 shown in Figure 18.EMC substrate 19 is fixed with two lead-in wires, one end of these lead-in wires are positioned at the central part of substrate, and the other end is drawn out to grid for welding when outside is installed to circuit card.Placed the chip 14 of blue light-emitting in one end of the 3rd lead-in wire 12, the bottom surface that lower electrode and the below of chip 14 go between is connected with conductive resin, and upper electrode is connected with thin gold thread 15 with the 4th lead-in wire 13.
By the fluorescent material in embodiment 6 and Sr 2si 5n 8: Eu fluorescent material mixes according to the ratio of 6:1, the powder mixed is mixed in silica gel or epoxy resin with 15% mass concentration, with point gum machine, the fluorescent material 17 mixed and silica gel or epoxy resin 16 are coated on the top of chip 14, silica gel or epoxy resin 18 are used for fixing chip 14 and fluorescent material 17, and the effect of parts 20 is gone out by the luminous reflectance that chip 14 and fluorescent material 17 send.The present embodiment luminescent device 11 illuminating source used is the LED sending 390 ~ 490nm wavelength light, the yellow fluorescent powder of wavelength light and other luminescent materials between the logical and 530 ~ 590nm sent according to the excitation of 390 ~ 490nm, thus sends white light.Figure 19 is the spectrogram of luminescent device, and the colour rendering index of illuminating device is 79, and colour temperature is 2988K.
Embodiment 16
Fluorescent material in embodiment 3 is mixed in epoxy resin with 10% mass concentration, is then encapsulated in the illuminating device shown in Figure 16.The chromaticity coordinates of obtained device is (0.3206,0.3265), and colour temperature is 6089K, and colour rendering index is 76.1.
Embodiment 17
By the fluorescent material in embodiment 6 and SrSi 2o 2n 2: Eu fluorescent material mixes according to the ratio of 1:2, is mixed in silica gel or epoxy resin by the powder mixed with 10% mass concentration, with point gum machine by the fluorescent powder packaging that mixes in the illuminating device shown in Figure 18.The chromaticity coordinates of obtained device is (0.3112,0.3356), and colour temperature is 6546K, and colour rendering index is 75.1.
Embodiment 18
By the fluorescent material in embodiment 12 and SrSi 2o 2n 2: Eu fluorescent material mixes according to the ratio of 1:2, is mixed in silica gel or epoxy resin by the powder mixed with 8% mass concentration, with point gum machine by the fluorescent powder packaging that mixes in the illuminating device shown in Figure 18.The chromaticity coordinates of obtained device is (0.3101,0.3391), and colour temperature is 6581K, and colour rendering index is 76.9.
Embodiment 19
By the fluorescent material in embodiment 11 and Sr 2si 5n 8: Eu fluorescent material mixes according to the ratio of 6:1, is mixed in silica gel or epoxy resin by the powder mixed with 15% mass concentration, with point gum machine by the fluorescent powder packaging that mixes in the illuminating device shown in Figure 18.The chromaticity coordinates of obtained device is (0.4322,0.395), and colour temperature is 2928K, and colour rendering index is 90.3.
Embodiment 20
By the fluorescent material in embodiment 12 and SrSi 2o 2n 2: Eu and Sr 2si 5n 8: Eu fluorescent material mixes according to the ratio of 7:1:2, is mixed in silica gel or epoxy resin by the powder mixed with 12% mass concentration, with point gum machine by the fluorescent powder packaging that mixes in the illuminating device shown in Figure 18.The chromaticity coordinates of obtained device is (0.3633,0.3302), and colour temperature is 4148K, and colour rendering index is 93.8.
The chemical formula of embodiment 21 fluorescent material is Y 2.4ce 0.1sr 0.5al 4.5si 0.5o 12
Raw material is Y 2o 3(analytical pure), CeO 2(analytical pure), SrCO 3(analytical pure), Al 2o 3(analytical pure) and SiO 2(analytical pure).Mol ratio is 1.2:0.1:0.5:2.25:0.5, raw mill mixing is placed in alumina container, 4 hours are sintered at the temperature of 1550 DEG C, sintering atmosphere is nitrogen hydrogen mixed gas, powder after sintering is taken out from container, select to pulverize, classification is also the HCl treatment of 3 moles often liter by volumetric molar concentration, the median size of synthesized fluorescent material is adjusted to 15 μm, afterwards that fluorescent material is extremely neutral with distilled water repetitive scrubbing, and then fluorescent material is put in alumina container, reduce 4 hours at the temperature of 1400 DEG C, reducing atmosphere is hydrogen, required fluorescent material can be obtained.Ce in this embodiment 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12mol ratio be approximately the excitation and emission spectra that 5, Figure 20 is the yellow fluorescent powder obtained.Can be found out by this figure, meet Ce relative to other 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12molar ratio range be greater than 14 and be less than 300 embodiments, in the present embodiment, the luminous intensity of fluorescent material obviously reduces.

Claims (10)

1. a yellow fluorescent powder, is characterized in that: its chemical formula is A xz yce 3-x-ye md 5-mo 12wherein A is one or more elements in La, Y, Lu and Tb, Z is one or more elements in Zn, Mg, Ca, Sr and Ba, E is one or more elements in Al, In and Ga, D is one or both of Si and Ge, 0<x<3, x+y<3,4.8≤m<5, y+m=5.
2. yellow fluorescent powder according to claim 1, is characterized in that: in described chemical formula, 0<y≤0.2.
3. yellow fluorescent powder according to claim 1, is characterized in that: described chemical formulation material is A by chemical constitution 3al 5o 12with Z 3al 2d 3o 12the system solid solution that both are formed.
4. yellow fluorescent powder according to claim 3, is characterized in that: described chemical formulation material is Ce 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12the limit solid solution formed, wherein, Ce 3+the Y activated 3al 5o 12with Ce 3+the Sr activated 3al 2si 3o 12molar ratio range be greater than 10 and be less than 300.
5. yellow fluorescent powder as claimed in any of claims 1 to 4, is characterized in that: the median size of described chemical formulation material is 1 ~ 100 μm.
6. yellow fluorescent powder as claimed in any of claims 1 to 4, is characterized in that: the extent of fluorescence under the exciting of any one light of described chemical formulation material in ultraviolet, visible ray and electron rays is 500 ~ 600nm.
7. a preparation method for the yellow fluorescent powder in Claims 1-4 described in any one, is characterized in that comprising the steps:
Oxide compound, carbonate or oxyhydroxide containing A, Z, E, D and Ce element is taken as raw material according to stoichiometric ratio according to chemical formula, at 1000 ~ 1600 DEG C, 2 ~ 10h is sintered after mixing, select the powder after one or more method process sintering in pulverizing, classification and acid treatment method, to adjust median size to 1 ~ 100 μm of powder, be washed with distilled water to neutrality; Reductase 12 ~ 10h at 1000 ~ 1400 DEG C, namely obtains yellow fluorescent powder afterwards.
8. the luminescent device made of the yellow fluorescent powder according to any one of Claims 1-4, it is characterized in that: comprise above-mentioned yellow fluorescent powder and illuminating source, described illuminating source is to send the photodiode of 300 ~ 490nm wavelength light, laser diode or organic EL luminous element, the colour temperature of luminescent device is greater than 6000K, and colour rendering index is greater than 75.
9. luminescent device according to claim 8, is characterized in that: also include other fluorescent material, and the colour temperature of luminescent device is less than 4800K, and colour rendering index is greater than 85.
10. luminescent device according to claim 9, other fluorescent material described in it is characterized in that are one or more in following fluorescent material: (Ca, Sr, Ba) 2si 5n 8: Eu, (Ca, Sr) AlSiN 3: Eu, β-SiAlON:Eu, (Ba, Sr) Y 2si 2al 2o 2n 5: Eu, Ca 2alSi 3o 2n 5: Eu, Ba 3si 6o 12n 2: Eu, (Ca, Sr, Ba) Si 2o 2n 2: Eu, Li 2ca 2si 2o 7: Eu, Cs 2mgSi 5o 12: Eu, (Ca, Sr, Ba) 2siO 4: Eu, (Ca, Sr, Ba) 2mgSi 2o 7: Eu, (Ca, Sr, Ba) 3mgSi 2o 8: Eu, BaSi 2o 5: Eu, Ba 2zn 3si 3o 11: Eu, (Ca, Sr, Ba) 2al 2siO 7: Eu, CaZrSi 2o 7: Eu, (Ca, Sr, Ba) Al 2o 4: Eu, Sr 4al 14o 25: Eu, Lu 3al 5o 12: Ce, Ca 3sc 2si 3o 12: Ce, SrAl 2b 2o 7: Eu, Sr 2b 2o 5: Eu, Ca 2al 3o 6f:Eu, Na 2siF 6: Mn.
CN201310262528.1A 2013-06-27 2013-06-27 Yellow fluorescent powder and preparation method thereof and light emitting device using fluorescent powder Pending CN104250555A (en)

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