CN102115666A - Method for synthesizing white light source by exciting rare earth doped aluminum oxynitride fluorescent powder through laser - Google Patents
Method for synthesizing white light source by exciting rare earth doped aluminum oxynitride fluorescent powder through laser Download PDFInfo
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- CN102115666A CN102115666A CN2009102478642A CN200910247864A CN102115666A CN 102115666 A CN102115666 A CN 102115666A CN 2009102478642 A CN2009102478642 A CN 2009102478642A CN 200910247864 A CN200910247864 A CN 200910247864A CN 102115666 A CN102115666 A CN 102115666A
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Abstract
The invention relates to a method for synthesizing a white light source by exciting rare earth doped aluminum oxynitride fluorescent powder through laser, which is characterized by comprising the following steps of: doping rare earth elements in aluminum oxynitride (AlON) serving as a matrix to prepare different doped fluorescent powder; and mixing more than two kinds of synthesized fluorescent powder, and drying to prepare the white light source which emits white light under the excitation of a 950nm semiconductor laser, wherein the mass percentage concentration of oxide doped with a rare earth element such as Er, Tm, Ho, Tb, Pr, Eu, Dy and Sm is 1 to 10 percent and the mass percentage concentration of oxide doped with a rare earth element Yb is 0.5 to 5 percent. The method comprises the following steps of: a) preparing an aluminum oxynitride matrix; b) preparing the fluorescent powder; and c) synthesizing the white light source. The fluorescent powder has high luminous intensity, and is more stable than the traditional fluoride; and the doped AlON emits white light under the excitation of laser with the wavelength of 980nm.
Description
Technical field
The present invention relates to a kind of preparation method of white light source, relate to a kind of method or rather, belong to the field of light emitting materials in the shiner Neo-Confucianism with the rare earth ion doped aluminum oxynitride fluorescent material of laser excitation synthesize white light light source.
Background technology
Since the nineties in 20th century, along with the exploitation of white light LEDs, LED from the special source field such as application such as large screen display, pilot lamp step into general illumination gradually and become illumination light source of new generation, LED subject matter is that cost is too high and brightness is on the low side at present.For obtaining the light source of enough brightness, need combination dozens of and even up to a hundred luminescence units usually.Obviously, except that improving production technique and using the more cheap semiconductor material, the luminous efficiency and the output rating that promote individual devices have become the effective way the most that reduces cost.People such as U.S. Ducharme propose a new method, replace LED to realize white light source (Ducharme et al., US patent 7088040,2006) with laser diode (LD).Compare with LED, LD is except that having the characteristics identical with LED, and it is good also to have the direction of light of sending, and therefore the energy density height more likely realizes high brightness and even super brightness white light.In addition, the LD technology is with respect to high-brightness LED, and its development is ripe relatively, does not have big technical difficulty, and this also is an important factor in order quickening industrialization.Can expect that following LD will constitute the core of lighting source of new generation with LED.
Realize using the adulterated fluorescent material of single LD excitation rare-earth to send red (R), green (G) at the fluorescent material of monochromatic LD surface applied or deposition different colours, blue (B) three primary colours light mixes, by regulating the ratio of three primary colours, can obtain the white light of different-colour and high Di (CRI).Fluorescent material is made up of active ions and matrix two portions, and the former is a luminescence center, has determined the characteristics of luminescence of fluorescent material; The latter then is supporting body and dispersion medium.The matrix that tradition is used for laserable material mainly contains fluorochemical, oxyfluoride and other halogenide.The halogenide laser damage threshold is low, chemical stability and poor heat stability, to environment and atmosphere sensitivity; And fluorochemical is big for environment pollution.Therefore, oxide compound and oxynitride are subjected to more concern in recent years, aluminum oxynitride because have good chemistry and photochemical stability, phonon energy low, make it become the candidate material of luminous host, can expect by selecting suitable dopant ion, can in this system, obtain up-conversion luminescence.
Summary of the invention
The objective of the invention is to propose the rear-earth-doped method of a kind of laser excitation with aluminum oxynitride fluorescent material synthesize white light light source, this method technology is simple, cost is low, the diameter of particle that obtains about 0.5～5 μ m, even particle distribution, stable performance can apply or be deposited on the LD surface and realize white light output, is used for lighting field.
The invention is characterized in: it is to be matrix with the aluminum oxynitride, and doped with rare-earth elements is made different adulterated fluorescent material, the semiconductor laser that is formed in 950nm after the two or more fluorescent material mixing of synthetic, the drying is excited down launch white light at last; The oxide concentration of doped with rare-earth elements Er, Tm, Ho, Tb, Pr, Eu, Dy or Sm is oxide concentration 0.5～5wt% of 1～10wt%, doped with rare-earth elements Yb.Particle diameter 0.5～5 μ m of the fluorescent material that is provided.
Provided by the present invention rare earth ion doped be that the fluorescent material of matrix adopts carbothermal reduction-nitridation method and solid reaction process preparation technology with the aluminum oxynitride, main raw material is Al
2O
3, carbon black, Er
2O
3, Tm
2O
3, Yb
2O
3, Ho
2O
3, Tb
2O
3, Pr
2O
3, Eu
2O
3, Dy
2O
3Or Sm
2O
3Rare earth oxide, uses alcohol solvent to be chemical pure at the purity of the purity of described rare earth oxide＞99.99%, aluminum oxide＞99.97%.
The present invention implements by following technological process:
The preparation of 1 matrix powder: mix with carbon black alumina powder jointed, carbon black accounts for 4.0～6.0wt% of mixed powder.The dried even back that is mixed is crossed the 200 mesh sieves corundum crucible of packing into and carry out reduction nitridation reaction in the flowing nitrogen atmosphere.Reaction is carried out in two steps: 1550 ℃ of insulation 1h are raised to 1650 ℃～1820 ℃ insulation 4～6h again.
The preparation of 2 fluorescent material powders: rare earth oxide and step 1 preparation aluminum oxynitride powder is incorporated with in the nylon ball grinder of aluminum oxide and mixes 2-5h, dispersion medium is an ethanol, alumina balls: powder: ethanol=5: 1: 1 (mass ratio).Compound is placed in the baking oven 60～120 ℃ of dry 12h under air conditions.Powder after the final drying, the sintering velocity with 3～8 ℃ under nitrogen atmosphere is warming up to 1800 ℃～1900 ℃ and insulation, furnace cooling then.
3 white light sources synthetic: it is even that the two or more fluorescent material of step 2 preparation is joined in the ethanol vigorous stirring, obtains mixed powder at 60～120 ℃ of dry 12h of baking oven then, evenly dried soft-agglomerated to break with the grinding of mill alms bowl.
The method of a kind of rare earth ion doped aluminum oxynitride fluorescent material synthesize white light light source provided by the invention has the following advantages:
1. rare earth ion doped aluminum oxynitride base fluorescent powder provided by the present invention has higher luminous intensity, and the fluorochemical that chemical property is more traditional is stable;
2. by selecting different dopant ion, codoped rare earth ion and different dopant ion concentration, ir radiation at the 980nm wavelength excites down, can make aluminum oxynitride fluorescent material after the doping realize the luminous of blue, green, red, yellow multiple different colours, mix two kinds then, realize white light output more than three kinds or three kinds;
3. owing to adopt carbothermic method to prepare the aluminum oxynitride powder, this method cost is low, purity is high, granularity is little.Can guarantee the even doping of rare earth ion again by the liquid-phase mixing method, high temperature solid-state method preparation technology is simple, and the diameter of particle that obtains is evenly distributed, and granular size is 0.5～5 μ m, need not specific installation, is convenient to scale operation.The powder that is provided mixes the back and realizes white light output, is used for lighting field.
Description of drawings
Fig. 1 is that the XRD crystalline phase of the sample behind the sintering is analyzed.Diffraction peak among the figure is all corresponding with cube aluminum oxynitride diffraction peak, does not have other miscellaneous appearance.
Fig. 2 is the stereoscan photograph of sample.As seen from the figure, the even particle distribution of powder, particle size are about 1～2 μ m.
Fig. 3 is embodiment 1 described Er
2O
3Doping aluminum oxynitride powder is a spectrum under the semiconductor laser of 980nm excites at emission wavelength.
Fig. 4 is embodiment 1 described Yb
2O
3, Er
2O
3Codoped aluminum oxynitride powder is a spectrum under the semiconductor laser of 980nm excites at emission wavelength.
Fig. 5 is white-light spectrum under the semiconductor laser of 980nm excites for embodiment 1 described mixed powder at emission wavelength.
Embodiment
Embodiment 1
At first with 96 gram Al
2O
3, the dried even back that is mixed of 4 gram carbon blacks crosses 200 mesh sieves.Pack into then and in the flowing nitrogen atmosphere, carry out the carbothermal reduction-nitridation reaction in the corundum crucible.Reaction is carried out in two steps: 1550 ℃ of insulation 1h, be raised to 1650 ℃ of insulation 2h again, and obtain the single-phase powder of AlON (as shown in Figure 1).Furnace cooling takes out powder, and second step is with the Er of 0.2 gram
2O
3With above-mentioned 10 the gram aluminum oxynitrides put into contain be equipped with 50 the gram alumina balls nylon ball grinder, add 10ml ethanol again and do dispersion agent, on ball mill, mix 2h.80 ℃ of dry 12h under the air conditions in baking oven.Dried powder is put into 1800 ℃ of insulations of multifunctional sintering furnace 4h, obtain Er
3+Adulterated aluminum oxynitride (AlON:Er
3+) powder.This diameter of particle is 1～2 μ m, even particle distribution, as shown in Figure 2.Under exciting, the semiconductor laser of 980nm launches bright orange-yellow fluorescence, as shown in Figure 3, this fluorescent material is spectrum under the semiconductor laser of 980nm excites at wavelength, and two main emission bands of green glow and ruddiness are arranged among the figure, peak emission wavelength is positioned at 548nm and 666nm, respectively correspondence and Er
3+Ionic
4S
3/2/
2H
11/2→
4I
15/2With
4F
9/2→
4I
15/2Energy level transition.The 3rd step is with the Tm of 0.05 gram
2O
3With 0.02 gram Yb
2O
3Put into the nylon ball grinder that contains 50 gram alumina balls with above-mentioned 10 gram aluminum oxynitrides, repeat above operation and obtain Tm
3+And Yb
3+Aluminum oxynitride (the AlON:Tm that mixes altogether
3+, Yb
3+) the fluorescent material powder.This fluorescent powder can excite at the semiconductor laser of 980nm launches bright blue-fluorescence down, as shown in Figure 4, this fluorescent material powder is a spectrum under the semiconductor laser of 980nm excites at wavelength, two main emission bands of blue light and ruddiness are arranged among the figure, peak emission wavelength is positioned at 479nm and 653nm, respectively correspondence and Tm
3+Ionic
1G
4→
3H
6With
1G
4→
3F
4Energy level transition.The 4th step was that two kinds of fluorescent material that step 2 and step 3 make are mixed to join in the ethanol vigorous stirring is even, then at 60～120 ℃ of dry 12h of baking oven.Under the semiconductor laser of 980nm excites, launch white light, see Fig. 5.
Embodiment 2
At first, with 94.4 gram Al
2O
3, the dried even back that is mixed of 5.6 gram carbon blacks crosses 200 mesh sieves.Pack into then and in the flowing nitrogen atmosphere, carry out the carbothermal reduction-nitridation reaction in the corundum crucible.Reaction is carried out in two steps: 1550 ℃ of insulation 1h, be raised to 1750 ℃ of insulation 3h again, and obtain the single-phase powder of AlON.Furnace cooling takes out powder, and second step was the H with 0.35 gram
2O
3Yb with 0.2 gram
2O
3Put into the nylon ball grinder that contains 50 gram alumina balls with 10 gram aluminum oxynitrides of the first step preparation, add 10ml ethanol and do dispersion agent, on ball mill, mix 5h.80 ℃ of dry 12h under the air conditions in baking oven.Dried powder is put into 1850 ℃ of insulations of multifunctional sintering furnace 4h, obtain AlON:Ho
3+, Yb
3+Powder.This diameter of particle is 1～2 μ m, even particle distribution.Under exciting, the semiconductor laser of 980nm launches bright orange-yellow fluorescence.The 3rd step was the Tm with 0.12 gram
2O
3With 0.02 gram Yb
2O
3The 10 gram aluminum oxynitrides that make with the first step are equipped with in the nylon ball grinder of 50 gram alumina balls, and the second step process method that repeats obtains AlON:Tm
3+, Yb
3+Powder.Under exciting, the semiconductor laser of 980nm launches bright blue-fluorescence; With the 4th step is that two kinds of fluorescent material that step 2 and step 3 make are mixed to join in the ethanol vigorous stirring is even, then at 100 ℃ of dry 12h of baking oven.Under exciting, the semiconductor laser of 980nm launches white light.
Embodiment 3
At first, with 94 gram Al
2O
3, the dried even back that is mixed of 6 gram carbon blacks crosses 200 mesh sieves.Pack into then and in the flowing nitrogen atmosphere, carry out the carbothermal reduction-nitridation reaction in the corundum crucible.Reaction is carried out in two steps: 1550 ℃ of insulation 1h, be raised to 1820 ℃ of insulation 4h again, and obtain the single-phase powder of AlON.Furnace cooling takes out powder; The 2nd step was the Er with 0.5 gram
2O
3Put into the nylon ball grinder that contains 50 gram alumina balls with 10 gram aluminum oxynitrides of the 1st step preparation, add 10ml ethanol and do dispersion agent, on ball mill, mix 2h, 80 ℃ of dry 12h under the air conditions in baking oven.Dried powder is put into 1900 ℃ of insulations of multifunctional sintering furnace 4h, obtain AlON:Er
3+Powder, this diameter of particle are 1～2 μ m, even particle distribution.Under exciting, the semiconductor laser of 980nm launches bright red fluorescence; The 3rd step is with the Tm of 0.2 gram
2O
3With 0.02 gram Yb
2O
3The 10 gram aluminum oxynitrides that prepare gained with the first step are equipped with in the nylon ball grinder of 50 gram alumina balls, and the technology that repeats above step 2 obtains AlON:Tm
3+, Yb
3+Powder.Under exciting, the semiconductor laser of 980nm launches bright blue-fluorescence.The 4th step is with the Ho of 0.12 gram
2O
3With 0.2 gram Yb
2O
3Put into the nylon ball grinder that contains 50 gram alumina balls with the 10 gram aluminum oxynitrides that step 1 makes, the technology that repeats above step 2 obtains AlON:Ho
3+, Yb
3+Powder.Under exciting, the semiconductor laser of 980nm launches bright green fluorescence.The 5th step be with above-mentioned steps 2,3 and 4 prepared three kinds of fluorescent material to be mixed to join in the ethanol vigorous stirring even, then at 100 ℃ of dry 12h of baking oven.Under exciting, the semiconductor laser of 980nm launches white light.
Claims (9)
1. the method for the rear-earth-doped aluminum oxynitride fluorescent material of laser excitation synthesize white light light source, it is characterized in that with the aluminum oxynitride being matrix, doped with rare-earth elements is made different adulterated fluorescent material, the semiconductor laser that is formed in 950nm after the two or more fluorescent material mixing of synthetic, the drying is excited down launch white light at last;
The oxide mass percentage concentration of described doped with rare-earth elements Er, Tm, Ho, Tb, Pr, Eu, Dy or Sm is 1-10%, and the mass percentage concentration of the oxide compound of doped with rare-earth elements Yb is 0.5-5%.
2. by the method for the described synthesize white light light source of claim 1, it is characterized in that may further comprise the steps:
A) preparation of aluminum oxynitride matrix
With Al
2O
3Powder mixes with carbon black, and dried sieve after the even crucible of packing into of being mixed divided for two steps carried out reduction reaction under the flowing nitrogen atmosphere, 1550 ℃ of the first steps, and second step was 1650-1820 ℃ to insulation 1h then; Insulation 4-6h;
B) preparation of fluorescent material powder
With the aluminum oxynitride powder of rare earth oxide in described ratio of claim 1 and step a preparation, be that dispersion medium is put in the nylon ball grinder of salic ball and mixed with ethanol, mix the 60-120 ℃ of oven dry in back, under nitrogen atmosphere, be warming up to 1800-1900 ℃ of insulation at last, be prepared into the doping aluminum oxynitride fluorescent material of different ions and different dopings;
C) white light source is synthetic
Two kinds of step b preparation, fluorescent material more than three kinds or three kinds are joined in the ethanolic soln, at 60-120 ℃ of dry 12h, promptly synthesize under 980nm laser excitation and launch white light then.
3. by the method for claim 1 or 2 described synthesize white light light sources, the particle diameter that it is characterized in that described fluorescent material is 0.5-5 μ m.
4. by the method for the described synthesize white light light source of claim 2, it is characterized in that purity＞99.99% of the rare earth oxide that uses, alumina powder jointed purity＞99.97% is a chemical pure as the ethanol of solvent.
5. by the method for the described synthesize white light light source of claim 2, it is characterized in that Al among the step a
2O
3To account for the mass percent of mixed powder be 4-6% to carbon black when mixing with carbon black.
6. by the method for the described synthesize white light light source of claim 2, the mass ratio when it is characterized in that mixing in the ball grinder among the step b between oxidation ball, powder and the ethanol is 5: 1: 1.
7. by the method for the described synthesize white light light source of claim 2, it is characterized in that step b synthetic Er
3+The fluorescent material of adulterated AlON matrix has two main emission bands of green glow and ruddiness, synthetic Tm under the semiconductor laser of 980nm excites
3+And Yb
3+The fluorescent material of the AlON matrix of mixing altogether has two main emission bands of blue light and ruddiness under the semiconductor laser of 980nm excites, above-mentioned two kinds of fluorescent material are launched white light under the semiconductor laser of 980nm excites after step c mixes.
8. by the method for the described synthesize white light light source of claim 2, it is characterized in that HO
3+And Yb
3+The fluorescent material of the AlON matrix of mixing is altogether launched orange-yellow fluorescence under the semiconductor laser of 980nm excites; Tm
3+And Yb
3+The fluorescent material of the AlON matrix of mixing is altogether launched blue-fluorescence under the semiconductor laser of 980nm excites, above-mentioned two kinds of fluorescent material are launched white light under the semi-conductor of 980nm excites after step c mixes.
9. by the method for the described synthesize white light light source of claim 2, it is characterized in that Er
3+The fluorescent material of adulterated AlON matrix is launched red fluorescence under the semiconductor laser of 980nm excites; Tm
3+And Yb
3+The fluorescent material of the AlON matrix of mixing is altogether launched blue light fluorescence under the semiconductor laser of 980nm excites; HO
3+And Yb
3+The fluorescent material of the AlON matrix of mixing is altogether launched green glow under the semiconductor laser of 980nm excites, above-mentioned three kinds of fluorescent material are launched white light under the semi-conductor of 980nm excites after step c mixes.
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