CN103045258A - Red fluorescent powder for white LED and preparation method thereof - Google Patents
Red fluorescent powder for white LED and preparation method thereof Download PDFInfo
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- CN103045258A CN103045258A CN2012105459912A CN201210545991A CN103045258A CN 103045258 A CN103045258 A CN 103045258A CN 2012105459912 A CN2012105459912 A CN 2012105459912A CN 201210545991 A CN201210545991 A CN 201210545991A CN 103045258 A CN103045258 A CN 103045258A
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Abstract
The invention discloses red fluorescent powder for a white light-emitting diode (LED) and a preparation method thereof. The red fluorescent powder for the white LED is prepared by co-doping rare earth elements and adjusting the formula of the fluorescent powder and by a high-temperature solid phase method. The preparation process is simple, the reaction condition is easy to control, and the obtained powder is pure in phase and uniform in particle appearance. The fluorescent powder shows excellent red luminescent property, has excellent luminescent intensity and can greatly improve the color development performance of the white LED. The heat stability of the red fluorescent powder at high temperature is more excellent than that of yttrium aluminium garnet fluorescent powder and the chemical properties of the red fluorescent powder are very stable, so the assembling requirement of the white LED with high brightness and high color development performance can be met and wide market prospect is achieved.
Description
Technical field
The present invention relates to LED fluorescent material field, particularly a kind of red fluorescent powder for white radiation LED and preparation method thereof.
Background technology
White light LEDs (Light Emitting Diode) has that energy consumption is low, volume is little, pollution-free, the characteristics such as luminous efficiency is high, the life-span is long and speed of reaction is fast, and its luminous efficiency has surpassed 150lm/W, is considered to the energy-conserving and environment-protective light source of a new generation.At present the white light LEDs technology of main flow is to utilize the blue-light excited yellow fluorescent powder of LED chip emission and realize white light emission.Being used for the most ripe fluorescent material of white light LEDs is YAG:Ce
3+Gold-tinted fluorescent material, but owing to lack the ruddiness composition, the colour rendering index of the white light LEDs that only encapsulates out with YAG is not high, is difficult to make the white light LEDs of low colour temperature.
The development of red fluorescence powder has been subjected to domestic and international researchist's extensive concern.Known luminescent material take aluminosilicate as matrix has good thermostability and chemical stability, the characteristics such as have that water tolerance is strong, the UV resistant radiation characteristic is good, luminous efficiency is high and glow color is various; YAG:Ce
3+The fluorescent material of garnet structure can produce larger crystal field advantage, has good thermal conductivity and physical strength, and anti-high intensity radiation and electronics bombardment be widely used as substrate material, and Ce are found in research
3+Emmission spectrum can realize red shift by increasing the covalency atom.How to prepare and granular, subsphaeroidal and and the YAG:Ce of axle such as have
3+The aluminosilicate fluorescent powder that processing performance approaches is people's problems of concern always.
Summary of the invention
The object of the present invention is to provide a kind of red fluorescent powder for white radiation LED and preparation method thereof.
The technical solution used in the present invention is:
A kind of red fluorescent powder for white radiation LED, the chemical constitution formula of this fluorescent material are (Y
3-x-y-zM
y) MgAl
3SiO
12: Ce
x, Pr
z, wherein M is a kind of among La, Tb, the Gd, 0≤x≤0.1,0≤y≤1.2,0≤z≤0. 01.
Preferably, in the chemical constitution formula of fluorescent material: 0.04≤x≤0.08,0.6≤y≤1,0.002≤z≤0.006.
A kind of preparation method of red fluorescent powder for white radiation LED may further comprise the steps:
1) chemical constitution formula according to red fluorescence powder takes by weighing each raw material;
2) mix each raw material, after the interpolation solvent carries out the wet mixing ball milling, take out product, dry, sieve, obtain the precursor powder;
3) add fusing assistant in the precursor powder, mix, under reducing atmosphere, 1300～1500 ℃ of insulation 3～6h obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder;
The chemical constitution formula of red fluorescence powder as claimed in claim 1 or 2.
Preferably, in the described raw material of step 1), the raw material of each metallic element is selected from its oxide compound, oxyhydroxide, carbonate or oxalate; The raw material of element silicon is silicon-dioxide.
Preferably, step 2) in, described solvent is at least a in water, ethanol, acetone, the ether.Preferably, the mass volume ratio of raw material and solvent (g/ml) is 1:(2～4).
Preferably, step 2) in, behind wet mixing ball milling 2～4h, take out product.
Preferably, above-mentioned fusing assistant is boric acid, BaF
2, NH
4At least a among F, the LiF.Preferably, fusing assistant is 0.1～5% of each raw material gross weight.
Preferably, described reducing atmosphere is nitrogen and hydrogen mixture, ammonia or carbon monoxide.
The invention has the beneficial effects as follows:
The present invention forms by the prescription of codoped rare earth element and adjustment fluorescent material, makes red fluorescent powder for white radiation LED, and fluorescent powder demonstrates good red luminous performance, and has good luminous intensity, can greatly improve the color developing of white light LEDs;
The present invention adopts high temperature solid-state method to prepare red fluorescent powder for white radiation LED, and technique is simple, and reaction conditions is easy to control, and the phase of gained powder is pure, and granule-morphology is even;
The thermal stability of red fluorescence powder of the present invention is better than yttrium aluminium garnet fluorescent powder, and its chemical property is highly stable, is better than silicate fluorescent powder, can satisfy the needs of high brightness, high-color rendering energy white-light LED encapsulation, has very wide market outlook.
Description of drawings
Fig. 1 is the utilizing emitted light spectrogram (λ of different samples among the embodiment 1
Ex=460nm);
Fig. 2 is the utilizing emitted light spectrogram (λ of different samples among the embodiment 2
Ex=460nm);
Fig. 3 is the utilizing emitted light spectrogram (λ of different samples among the embodiment 3
Ex=460nm);
Fig. 4 is the utilizing emitted light spectrogram (λ of different samples among the embodiment 4
Ex=460nm);
Fig. 5 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004XRD figure;
Fig. 6 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004SEM figure;
Fig. 7 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004The thermal quenching performance map.
Embodiment
A kind of red fluorescent powder for white radiation LED:
A kind of red fluorescent powder for white radiation LED, the chemical constitution formula of this fluorescent material are (Y
3-x-y-zM
y) MgAl
3SiO
12: Ce
x, Pr
z, wherein M is a kind of among La, Tb, the Gd, 0≤x≤0.1,0≤y≤1.2,0≤z≤0. 01.
Preferably, in the chemical constitution formula of fluorescent material: 0.04≤x≤0.08,0.6≤y≤1,0.002≤z≤0.006.
More excellent, the chemical constitution formula of this fluorescent material is Y
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004Its emission main peak is positioned at about 610nm, is a kind of LED red fluorescence powder of high brightness.
A kind of preparation method of red fluorescent powder for white radiation LED may further comprise the steps:
1) chemical constitution formula according to red fluorescence powder takes by weighing each raw material;
2) mix each raw material, after the interpolation solvent carries out the wet mixing ball milling, take out product, dry, sieve, obtain the precursor powder;
3) add fusing assistant in the precursor powder, mix, under reducing atmosphere, 1300～1500 ℃ of insulation 3～6h obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder;
The chemical constitution formula of red fluorescence powder as claimed in claim 1 or 2.
Preferably, in the described raw material of step 1), the raw material of each metallic element is selected from its oxide compound, oxyhydroxide, carbonate or oxalate, is not advisable not introduce other impurity behind the high temperature sintering, take its oxide compound as example, but is not limited to this among the embodiment; The raw material of element silicon is preferably silicon-dioxide.
Preferably, step 2) in, described solvent is at least a in water, ethanol, acetone, the ether.Preferably, the mass volume ratio of raw material and solvent (g/ml) is 1:(2～4).
Preferably, step 2) in, behind wet mixing ball milling 2～4h, take out product.
Preferably, above-mentioned fusing assistant is boric acid, BaF
2, NH
4At least a among F, the LiF.Preferably, fusing assistant is 0.1～5% of each raw material gross weight.
Preferably, described reducing atmosphere is nitrogen and hydrogen mixture, ammonia or carbon monoxide.
Below in conjunction with embodiment, further set forth the present invention.
Embodiment 1
1) at first according to the chemical constitution formula of fluorescent material, take by weighing various raw materials according to stoichiometric ratio, the quality of each raw material is as shown in table 1:
2) mix above-mentioned raw materials, add water and mix, raw material is 1:2 with the volume mass of water than (g/ml), and behind the wet mixing ball milling 3h, suction filtration is dried, sieved, and obtains the precursor powder;
3) add fusing assistant boric acid in the precursor powder, grind evenly with mortar, the weight of fusing assistant is 0.5% of raw material gross weight; Then nitrogen and hydrogen mixture atmosphere (volume ratio N in the high-temperature tubular atmosphere furnace
2: H
2=reduce sintering under 95:5), behind 1420 ℃ of insulation 4h, obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder.
Fig. 1 is the utilizing emitted light spectrogram of each sample among the embodiment 1, namely works as Y
3-xMgAl
3SiO
12: Ce
x 3+The doping x of middle Ce gets respectively one group of utilizing emitted light spectrogram of 0.04,0.06,0.08,0.1 o'clock.As can be seen from Figure 1, along with the increase of Ce doping, the brightness of fluorescent material strengthens gradually, and emission wavelength generation red shift, and when x=0.06, the luminous intensity of powder reaches optimum value; The afterwards continuation along with Ce content increases, and the concentration quenching phenomenon appears in powder.Therefore, in subsequent embodiment, the equal value of x is 0.06.
Embodiment 2
1) at first according to the chemical constitution formula of fluorescent material, take by weighing various raw materials according to stoichiometric ratio, the quality of each raw material is as shown in table 2:
2) mix above-mentioned raw materials, add acetone and mix, the mass volume ratio of raw material and acetone (g/ml) is 1:3, and behind the wet mixing ball milling 2h, suction filtration is dried, sieved, and obtains the precursor powder;
3) in the precursor powder, add fusing assistant BaF
2, being ground, the weight of fusing assistant is 1% of raw material gross weight; Then nitrogen and hydrogen mixture atmosphere (volume ratio N in the high-temperature tubular atmosphere furnace
2: H
2=reduce sintering under 95:5), behind 1400 ℃ of insulation 4h, obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder.
Fig. 2 is the utilizing emitted light spectrogram of each sample among the embodiment 2.Can find out that in conjunction with Fig. 1 and table 3 when undoping other rare earth element, namely fluorescent material consists of Y
2.94MgAl
3SiO
12: Ce
0.06The time, its emission main peak is positioned at the 553nm place; When mixing different rare earth Gds, Tb, La, further red shift all occurs in the emission main peak of fluorescent material, and its main peak lays respectively at 578,560, the 565nm place; Doping Tb, along with main peak moves toward the long wave direction, the luminous intensity of fluorescent material reduces greatly during La; And the red shift of doping Gd time emission main peak also has higher luminous intensity to the 578nm place.The characteristics of luminescence index of comprehensive each sample finds to have preferably luminescent properties and so that fluorescent material main peak red shift when Gd partly replaces Y.
Embodiment 3
1) at first according to the chemical constitution formula of fluorescent material, take by weighing various raw materials according to stoichiometric ratio, the quality of each raw material is as shown in table 4:
2) mix above-mentioned raw materials, add ethanol and mix, the mass volume ratio of raw material and ethanol (g/ml) is 1:4, and behind the wet mixing ball milling 3h, suction filtration is dried, sieved, and obtains the precursor powder;
3) in the precursor powder, add fusing assistant NH
4F grinds evenly with mortar, and the weight of fusing assistant is 5% of raw material gross weight; Then in the high-temperature tubular atmosphere furnace, reduce sintering under the ammonia atmosphere, behind 1350 ℃ of insulation 4h, obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder.
Fig. 3 is the utilizing emitted light spectrogram of each sample among the embodiment 3, i.e. the utilizing emitted light spectrogram of one group of sample when the doping y of doped rare earth element Gd gets respectively 0.4,0.6,0.8,1.0,1.2 altogether.As can be seen from Figure 3, along with the increase of Gd doping, emission peak moves toward the long wave direction, and brightness reduces gradually.When y=1.0, the emission peak red shift is to the 605nm and can keep higher luminous intensity, and when the Gd amount was increased to 1.2, the luminous intensity of powder reduced greatly, so the optimum doping amount of Gd is 1.0.
Embodiment 4
1) at first according to the chemical constitution formula of fluorescent material, take by weighing various raw materials according to stoichiometric ratio, the quality of each raw material is as shown in table 5:
2) mix above-mentioned raw materials, add ether and mix, the mass volume ratio of raw material and ether (g/ml) is 1:3, and behind 25 ℃ of lower wet mixing ball milling 4h, suction filtration is dried, sieved, and obtains the precursor powder;
3) add fusing assistant LiF in the precursor powder, grind evenly with mortar, the weight of fusing assistant is 2% of raw material gross weight; Then in the high-temperature tubular atmosphere furnace, reduce sintering under the carbon monoxide atmosphere, behind 1450 ℃ of insulation 5h, obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder.
Fig. 4 is the utilizing emitted light spectrogram of embodiment 4 different samples, namely at chemical constitution formula Y
1.94-zGdMgAl
3SiO
12: Ce
0.06, Pr
zIn, the utilizing emitted light spectrogram of one group of sample when z gets respectively 0.002,0.004,0.006,0.008,0.01.As seen from Figure 4, when doping Pr, Pr appears about 611nm
3+The characteristic emission peak, increased red ratio, improved color developing; And (sample composition is Y when z=0.004
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004), the luminous intensity of sample is the highest, can be used as a kind of good LED red illuminating material.
Fig. 5 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004XRD figure.As can be seen from the figure its spectrogram and standard card are basically identical, illustrate that doping Gd, Pr do not affect the crystalline phase of powder, adopt the fluorescent material phase of this method preparation very pure.
Fig. 6 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004SEM figure.As can be seen from Figure, adopt the made powder granule of this technology size evenly, be spherical particle, and size-grade distribution concentrates, its medium particle diameter is about 10 μ m.
Fig. 7 is sample Y among the embodiment 4
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004The thermal quenching performance map.Because the rising of temperature causes commercial YAG and (Y
1.936,Gd) MgAl
3SiO
12: Ce
0.06Pr
0.004Luminescent properties deteriorated, as can be seen from Figure, when being elevated to 300 ℃ along with temperature by 25 ℃, YAG and (Y
1.936,Gd) MgAl
3SiO
12: Ce
0.06,Pr
0.004All decreases to some degree of luminous intensity, but Y comparatively speaking
1.936GdMgAl
3SiO
12: Ce
0.06Pr
0.004Changing down is slower, illustrates that its thermal stability at high temperature is better than YAG.
Conventional yttrium aluminium garnet fluorescent powder thermal stability at high temperature is relatively poor, and the brightness quencher is fast; And silicate fluorescent powder since easily the moisture absorption and easily and airborne moisture react its poor chemical stability.The present invention take aluminosilicate as matrix, with Ce
3+Be activator, prepared red fluorescent powder for white radiation LED by high temperature solid-state method, and further form by the prescription of adjusting fluorescent material, prepare the element La that mixed
3+, Tb
3+Or Gd
3+, and codoped rare earth activators Pr
3+Red fluorescence powder, the powder emission peak produces red shift, and possesses good luminous intensity.Red fluorescence powder of the present invention combines the feature performance benefit of yttrium aluminum garnet and silicate fluorescent powder, thermal quenching performance at high temperature obviously is better than the yttrium aluminium garnet fluorescent powder (see figure 7), and its chemical property is highly stable, in air atmosphere, do not decompose rotten, be difficult for reacting with airborne moisture, oxygen, carbonic acid gas etc., can satisfy the needs of high brightness, the assembling of high-color rendering energy white light LEDs, have very wide market outlook.
Claims (10)
1. red fluorescent powder for white radiation LED, the chemical constitution formula of this fluorescent material is (Y
3-x-y-zM
y) MgAl
3SiO
12: Ce
x, Pr
z, wherein M is a kind of among La, Tb, the Gd, 0≤x≤0.1,0≤y≤1.2,0≤z≤0. 01.
2. a kind of red fluorescent powder for white radiation LED according to claim 1 is characterized in that: in the chemical constitution formula of fluorescent material: 0.04≤x≤0.08,0.6≤y≤1,0.002≤z≤0.006.
3. the preparation method of a red fluorescent powder for white radiation LED may further comprise the steps:
1) chemical constitution formula according to red fluorescence powder takes by weighing each raw material;
2) mix each raw material, after the interpolation solvent carries out the wet mixing ball milling, take out product, dry, sieve, obtain the precursor powder;
3) add fusing assistant in the precursor powder, mix, under reducing atmosphere, 1300～1500 ℃ of insulation 3～6h obtain just powder;
4) first powder is carried out aftertreatment, obtain red fluorescence powder;
The chemical constitution formula of red fluorescence powder as claimed in claim 1 or 2.
4. preparation method according to claim 3, it is characterized in that: in the described raw material of step 1), the raw material of each metallic element is selected from its oxide compound, oxyhydroxide, carbonate or oxalate; The raw material of element silicon is silicon-dioxide.
5. preparation method according to claim 3 is characterized in that: step 2) in, described solvent is at least a in water, ethanol, acetone, the ether.
6. it is characterized in that according to claim 3 or 5 described preparation methods: the mass volume ratio of raw material and solvent (g/ml) is 1:(2～4).
7. preparation method according to claim 3 is characterized in that: step 2) in, behind wet mixing ball milling 2～4h, take out product.
8. preparation method according to claim 3, it is characterized in that: described fusing assistant is boric acid, BaF
2, NH
4At least a among F, the LiF.
9. it is characterized in that according to claim 3 or 8 described preparation methods: described fusing assistant is 0.1～5% of each raw material gross weight.
10. preparation method according to claim 3, it is characterized in that: described reducing atmosphere is nitrogen and hydrogen mixture, ammonia or carbon monoxide.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305219A (en) * | 2013-07-08 | 2013-09-18 | 常州化学研究所 | Yttrium aluminum garnet fluorescent powder for white light-emitting diode (LED) and preparation method thereof |
| CN113387568A (en) * | 2020-03-13 | 2021-09-14 | 包头稀土研究院 | Red fluorescent glass material and preparation method and application thereof |
-
2012
- 2012-12-14 CN CN201210545991.2A patent/CN103045258B/en active Active
Non-Patent Citations (5)
| Title |
|---|
| 《Journal of the American Ceramic Society》 20120731 Hongde Luo et al. Synthesis and Luminescence Properties of Mg-Si Co-doped Tb3Al5O12:Ce3+ Phosphors with Blue Excitation for White LEDs , * |
| HO SEONG JANG ET AL.: "Enhancement of red spectral emission intensity of Y3Al5O12:Ce3+ phosphor via Pr co-doping and Tb substitution for the application to white LEDs", 《JOURNAL OF LUMINESCENCE》 * |
| HONGDE LUO ET AL.: "Synthesis and Luminescence Properties of Mg–Si Co-doped Tb3Al5O12:Ce3+ Phosphors with Blue Excitation for White LEDs", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
| QIYUE SHAO ET AL.: "Temperature-dependent photoluminescence studies on Y2.93−xLnxAl5O12:Ce0.07(Ln=Gd, La) phosphors for white LEDs application", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| QIYUE SHAO ET AL.: "Temperature-dependent photoluminescence studies on Y2.93−xLnxAl5O12:Ce0.07(Ln=Gd, La) phosphors for white LEDs application", 《JOURNAL OF ALLOYS AND COMPOUNDS》, 25 March 2010 (2010-03-25) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305219A (en) * | 2013-07-08 | 2013-09-18 | 常州化学研究所 | Yttrium aluminum garnet fluorescent powder for white light-emitting diode (LED) and preparation method thereof |
| CN113387568A (en) * | 2020-03-13 | 2021-09-14 | 包头稀土研究院 | Red fluorescent glass material and preparation method and application thereof |
| CN113387568B (en) * | 2020-03-13 | 2022-03-18 | 包头稀土研究院 | Red fluorescent glass material and preparation method and application thereof |
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