CN1381547A - Vacuum ultraviolet excited green aluminate fluorescent powder and its preparing process - Google Patents

Vacuum ultraviolet excited green aluminate fluorescent powder and its preparing process Download PDF

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CN1381547A
CN1381547A CN 01110746 CN01110746A CN1381547A CN 1381547 A CN1381547 A CN 1381547A CN 01110746 CN01110746 CN 01110746 CN 01110746 A CN01110746 A CN 01110746A CN 1381547 A CN1381547 A CN 1381547A
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barium
raw material
vacuum ultraviolet
excited
fluorescent powder
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CN1219848C (en
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庄卫东
盛照昆
武杰
鱼志坚
韩钧祥
黄小卫
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

A green fluorescent aluminate powder has the chemical formula: BaxAl12-y-zMnyBzO19, where x=0.699-0.99, y=0.13-0.3 and z=0.001-0.1, and is prepared through proportioning, adding additive mixing by grinding, calcining at 1300-1450 deg.C for 2-10 hr under reduction condition, adding water, ball grinding to form slurry, washing with hot water, filtering by drowing and baking dry. Its advantages are high light intensity and low cost.

Description

A kind of aluminate green fluorescent powder of excited by vacuum ultraviolet and manufacture method thereof
The present invention relates to a kind of luminescent material and manufacture method thereof of excited by vacuum ultraviolet, the aluminate green fluorescent powder and the method for making thereof of the baric of more specifically saying so.
In recent years, plasma flat-plate shows that (plasma dispay panel is hereinafter to be referred as PDP) technology has obtained developing rapidly.PDP is that the vacuum ultraviolet ray (VUV) launched when utilizing noble gas discharge such as Xe or Xe-Ne excites the fluorescent material that is coated on the display screen and display image.In order to obtain the fluorescent material that panchromatic PDP need use three types of red, green, blues.The green emitting phosphor that PDP uses mainly contains Zn 2SiO 4: Mn and BaAl 12O 19: two kinds of Mn.Zn 2SiO 4: Mn will be eliminated gradually because time of persistence is oversize.BaAl 12O 19: Mn is because to have a time of persistence shorter, excites luminous byer force down vacuum ultraviolet, is easy to again synthesize, and low cost and other advantages is being applied gradually, will become one of fluorescent material that is used for PDP.
Along with the enhancing of people's environmental protection consciousness and the progress of China's " green illumination " engineering, rare gas discharge lamp has also obtained further development.Rare gas discharge lamp claims non-mercury florescent lamp again.Because it is without mercury, can reduce the pollution of mercury and to the harm of human and environment.This lamp is to utilize high-energy excited by vacuum ultraviolet fluorescent material that xenon gaseous discharge sends and alight, and the used fluorescent powder type of fluorescent material that this kind lamp is used and PDP seemingly.
The BaAl of 1 mole of routine 12O 19: the content of Ba is about 1 mole among the Mn, and Al is about 12 moles, about 0.12 mole of Mn.In order to adapt to the needs of PDP and rare gas discharge lamp, the luminosity of this fluorescent material needs further to improve.
American documentation literature US5,868,963 have reported a kind of new barium aluminate green emitting phosphor, and this fluorescent material is BazAl 12-xMnxO 19, wherein Z is 0.8～1.3,0.2＜X＜0.7.Its preparation method is by BazAl 12-xMnxO 19Take by weighing raw material aluminium sesquioxide, barium carbonate, manganous carbonate, with suspension mixing and stirring in mixing machine of raw material aluminium sesquioxide, barium carbonate, manganous carbonate.Behind the sieve that shakes, water evaporates is removed.The pulverulent mixture that obtains is put into alumina crucible, covers the crucible cover made from aluminium sesquioxide, puts into the stove of sealing, removes the air in the stove.In the atmosphere of exsiccant nitrogen or nitrogen and hydrogen, heating is 2 hours under 1400-1550 ℃ temperature.Product after the heat treated is the white powder of average grain 10 μ m.In the prescription of american documentation literature US 5,868,963, the content of manganese is brought up between 0.2～0.7.This is to attempt time of persistence of reducing the barium aluminate green emitting phosphor by the content that increases manganese.But, show that through our experiment manganese content increases too much, certainly will cause the reduction of fluorescent material brightness.Therefore, manganese content must be controlled at a moderate scope.Above-mentioned american documentation literature points out that also the optimum range of barium content is between 0.8～1.3.Experimental study through us shows that barium content is higher than at 1 o'clock, and the brightness of fluorescent material obviously descends.
Hong Guangyan etc. are in that " fusing assistant is to twinkler BaAl 12O 19: Mn structure and luminous influence (luminous journal, Vol20, No4,1999,311-315) " studied fusing assistant to BaAl in the literary composition 12O 19: the influence of Mn light-emitting phosphor brightness.The result shows H 3BO 3Be unfavorable for that it is luminous, AlF 3Little to its luminous raising, BaF 2Then can increase its luminous intensity significantly.
Purpose of the present invention is exactly on different components of further investigation and the basis of content to manganese activated barium aluminate green emitting phosphor performance impact thereof, a kind of new barium aluminate fluorescent material and manufacture method thereof are proposed, thereby improve the luminosity of this fluorescent material under excited by vacuum ultraviolet, in order to substitute existing BaAl 12O 19: Mn is applied in PDP or the rare gas discharge lamp.
Studies show that at BaAl 12O 19: add boric acid (H in the Mn fluorescent material 2BO 3) or boron trioxide (B 2O 3) and the fluorochemical of alkali metal halide or aluminium after the luminous intensity of fluorescent material is increased.Never add boron (B) or add in the contrast of X-ray diffractogram of boron (seeing Fig. 1 and Fig. 2), formed BaxAl after adding B as can be seen 12-y-zMnyBzO 19Fluorescent material.
The aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of the present invention, the chemical formula of this green emitting phosphor are BaxAl 12-y-zMnyBzO 19, 0.699≤x≤0.99,0.13≤y≤0.3,0.001≤z≤0.1 wherein.
The manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of the present invention,
1) presses chemical formula BaxAl 12-y-zMnyBzO 190.699≤x≤0.99 wherein, 0.13≤y≤0.3,0.001 prepare burden in≤z≤0.1, with wherein a kind of of barium oxide, barium salt is the raw material of barium, with wherein a kind of of aluminum oxide, hydrogen aluminum hydride, Burow Solution is the raw material of aluminium, is the raw material of manganese with wherein a kind of of Manganse Dioxide, manganese salt, is the raw material of boron with boron trioxide or boric acid.
2) add additive in batching, the amount of additive is to add 0.001～0.1 mole alkaline earth metal halide or the halogenide of aluminium or the halid mixture of alkaline earth metal halide and aluminium in every mole of fluorescent material.
3) will grind the even compound that forms that is mixed as the raw material of barium, the raw material of aluminium, the raw material of manganese, the raw material and the additive of boron.
4) under the reductive condition in 1300-1450 ℃ with compound calcination 2-10 hour, form firing product.
5) product of calcination is added water and carry out ball milling and form the powder slurry, wash, filter the back oven dry with hot water.Obtain the powder of body colour, become fluorescent material product of the present invention for white.
Said additive alkaline earth metal halide is barium fluoride (BaF 2), bariumchloride (BaCl 2) wherein a kind of, the halogenide of additive-aluminium is aluminum chloride (AlCl 3), aluminum fluoride (AlF 3) wherein a kind of.The mixture of halides of said additive alkaline earth metal halide and aluminium is barium fluoride (BaF 2) and aluminum fluoride (AlF 3) mol ratio be 1: 1 mixture.
Said barium salt is barium oxalate, barium carbonate, barium acetate a kind of barium salt wherein.Manganese salt is manganous carbonate, manganous oxalate, manganous sulfate a kind of manganese salt wherein.Will as the raw material of the raw material of the raw material of the raw material of barium, aluminium, manganese, boron and additive be dry grinded or water mill 4-15 hour, the mill even compound that forms that is mixed.The weight ratio of ball and all raw materials and additive total amount was 1: 0.5～1.5 when mill mixed.To grind mixed uniform compound places corundum crucible to carry out high temperature sintering.
When the content of manganese was higher in the fluorescent material, divalent manganesetion was easy to be oxidized to the more mn ion of high price such as trivalent or tetravalence.Therefore, in the process of carrying out the high temperature sintering compound, must under reductive condition, carry out.Said reductive condition can be after the mixed uniform compound of mill is placed corundum crucible (alumina crucible), after the layer of active carbon of the shop, surface of compound, to add the corundum crucible lid, carries out high temperature sintering again.Another kind of better reductive condition is to carry out high temperature sintering in the atmosphere (reducing atmosphere) of hydrogen atmosphere or nitrogen and hydrogen gas mixture.Need not add the corundum crucible lid when in hydrogen or nitrogen and hydrogen mixed gas atmosphere, carrying out high temperature sintering on the corundum crucible.The volume ratio of nitrogen and hydrogen is 1: 0.04～4 in the mixed gas of nitrogen and hydrogen.The flow that feeds hydrogen or nitrogen and hydrogen gas mixture is relevant with the size of stove.The flow that the used more small-sized High Temperature Furnaces Heating Apparatus of the present invention feeds hydrogen or nitrogen and hydrogen mixture is 8～15 milliliters/second.Preferably High Temperature Furnaces Heating Apparatus was vacuumized in the past feeding hydrogen or nitrogen and hydrogen gas mixture, to reduce the oxygen content in the stove.If in advance High Temperature Furnaces Heating Apparatus is not vacuumized, feeding hydrogen or nitrogen and hydrogen gas mixture before intensification, to drive time of air longer.In the atmosphere of the mixed gas of hydrogen or nitrogen and hydrogen (reductive condition) under 1300-1450 ℃ temperature with compound calcination 2-10 hour.To through 1300-1450 ℃, after the firing product after calcination 2-10 hour adds entry, carried out ball milling 1-5 hour, form the powder slurry, the water yield that is added is a firing product and the weight ratio of the water that is added is 1: 0.5～2.5.The weight ratio of ball and firing product is 1: 0.5～1.5 during ball milling.Powder slurry washs with hot water, washing to wash electrical conductivity of water constant till, generally with hot wash firing product 3-5 time for well.The weight ratio of firing product and water is 1: 3～5 during hot wash.Said hot water is the deionized water of heat, distilled water a kind of water wherein of heat, to filtering through the firing product after the hot wash.Product after the filtration is dried under 105-130 ℃ temperature, and forms the fluorescent material product of the present invention that body colour is a white.Said being filtered into filter paper filtering, suction filtration, press filtration, centrifuging a kind of method wherein.
The aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of the present invention and the advantage of manufacture method thereof just are:
1. propose the composition of new bivalent manganese activated barium aluminate green emitting phosphor, reduced calcination temperature, improved the luminous intensity of fluorescent material.
2. the manufacture method of barium aluminate fluorescent material of the present invention is simple, easy handling, and cost is low.
3. fluorescent material of the present invention transmitting green light under excited by vacuum ultraviolet can be used as the green composition of fluorescent material in PDP or the rare gas discharge lamp.
Fig. 1 BaxAl 12-yMnyO 19In do not add the X-ray diffractogram of B
Among the figure, ordinate zou is CPS (intensity), and X-coordinate is 2 θ angles, and used testing tool is Japanese D-MAX-RB X-ray diffraction analysis instrument of science, CuK α radiation, tube voltage: 40KV, tube current: 150mA.
Fig. 2 BaxAl 12-yMnyO 19X-ray diffractogram behind the middle adding B
Among the figure, ordinate zou is CPS (intensity), and X-coordinate is 2 θ angles, and used testing tool is Japanese D-MAX-RB X-ray diffraction analysis instrument of science, CuK α radiation, tube voltage: 40KV, tube current: 150mA.The amount that adds boron is 0.01 mole.
The spectral line peak value is offset to high angle add B as can be seen from the contrast of Fig. 1, Fig. 2 after, illustrates that B has entered in the structure of barium aluminate fluorescent material of the present invention.
Below with embodiment the aluminate green fluorescent powder and the manufacture method thereof of excited by vacuum ultraviolet of the present invention are further described; to help product of the present invention and manufacture method are done further to understand; protection scope of the present invention is not subjected to the qualification of these embodiment, and protection scope of the present invention is decided by claims.
Embodiment 1
The aluminate green fluorescent powder product of the excited by vacuum ultraviolet of present embodiment its chemical formula by analysis is Ba 0.799Al 11.840Mn 0.185B 0.007O 18.71X is 0.799, and y is 0.135, and z is 0.007.
Its manufacture method is for taking by weighing 0.8 mole of barium carbonate, aluminium sesquioxide (Al 2O 3) 5.925 moles, manganous carbonate (MnCO 3) 0.14 mole, boric acid (H 3BO 3) 0.01 mole as raw material.The amount of additive barium fluoride is to add 0.01 mole of barium fluoride in the fluorescent material of every Melbourne embodiment.
Will be as barium carbonate, aluminium sesquioxide, manganous carbonate, boric acid and the additive B aF of raw material 2Pack in the ball grinder, ball milling 12 hours forms the compound that mixes, and the weight ratio of agate ball amount and barium carbonate, aluminium sesquioxide, manganous carbonate, boric acid and barium fluoride total amount is 1: 1 during ball milling.
The compound that mixes is packed in the corundum crucible, the corundum crucible that fills compound is placed High Temperature Furnaces Heating Apparatus, feed the mixed gas of nitrogen and hydrogen, drive the air in the stove, the volume ratio of nitrogen and hydrogen is 1: 1.Heat up, in the reducing atmosphere of the mixed gas of nitrogen and hydrogen in 1450 ℃ of high temperature sinterings 3 hours.The flow of nitrogen and hydrogen is 11 milliliters/second.The product of calcination is packed in the ball grinder, add entry and high-quality glass sphere, the weight ratio of high-quality glass sphere and firing product is 1: 1.2, the water yield that is added by firing product with the weight ratio of the adding water yield be 1: 1.Carry out ball milling 2 hours, and formed the powder slurry.With hot deionized water wash 3 times of powder slurry, the weight ratio of each firing product and hot deionized water 1: 4.In baking oven, under 110 ℃ temperature, dried by the fire 12 hours behind the suction filtration, with its oven dry.Conventional BaAl 12O 19: the luminous intensity of the fluorescent material of Mn (seeing comparing embodiment) is 100% o'clock, and present embodiment gained fluorescent material relative luminous intensity under the 147nm excited by vacuum ultraviolet is 110%, and luminous intensity is apparently higher than comparing embodiment.
Comparing embodiment:
The chemical formula of comparing embodiment is BaAl 12O 19: Mn.
Take by weighing 0.99 mole of barium carbonate, 6 moles of aluminium sesquioxides, 0.12 mole of manganous carbonate be as raw material, and the amount of additive barium fluoride is to add 0.01 mole of BaF in the fluorescent material of every Melbourne comparing embodiment 2Its manufacture method is fully with embodiment 1, and the luminous intensity under the gained fluorescent material measuring condition identical with embodiment is 100%.
Embodiment 2-4
Its chemical formula by analysis of embodiment 2 is Ba 0.698Al 11.845Mn 0.136B 0.006O 18.608
Its chemical formula by analysis of embodiment 3 is Ba 0.899Al 11.835Mn 0.137B 0.008O 18.795
Its chemical formula by analysis of embodiment 4 is Ba 0.975Al 11.847Mn 0.136B 0.007O 18.887
By taking by weighing raw material and additive (adding 0.01 mole of barium fluoride in the fluorescent material of every mole of embodiment) shown in the table 1, all the other conditions are with embodiment 1.Gained fluorescent material intensity is listed in the table 1.When different barium content, the luminous intensity of embodiment 2-4 all is higher than comparing embodiment.
The raw material of table 1 embodiment 2-4, additive and luminous intensity embodiment raw material (mole) additive luminous intensity (%)
BaCO 3 Al 2O 3 MnCO 3 H 3BO 3?BaF 2
2 0.70 5.925 0.14 0.01 0.01 107
3 0.90 5.925 0.14 0.01 0.01 110
4 0.98 5.925 0.14 0.01 0.01 106
Embodiment 5-7
Its chemical formula by analysis of embodiment 5 is Ba 0.798Al 11.796Mn 0.195B 0.007O 18.683
Its chemical formula by analysis of embodiment 6 is Ba 0.799Al 11.752Mn 0.238B 0.008O 18.671
Its chemical formula by analysis of embodiment 7 is Ba 0.797Al 11.695Mn 0.297B 0.007O 18.642
(add 0.01 mole of BaF in the fluorescent material of every mole of embodiment by taking by weighing raw material and additive shown in the table 2 2), all the other conditions are with embodiment 1, and gained fluorescent material intensity is listed in the table 1.When different manganese content, the luminous intensity of embodiment 5-7 all is higher than comparing embodiment.
The raw material of table 2 embodiment 5-7, additive and luminous intensity embodiment raw material (mole) additive luminous intensity (%)
BaCO 3 Al 2O 3?MnCO 3 H 3BO 3?BaF 2 5 0.80 5.895 0.199 0.01 0.01 112 6 0.80 5.875 0.24 0.01 0.01 113 7 0.80 5.845 0.30 0.01 0.01 110
Embodiment 8-11
Its chemical formula by analysis of embodiment 8 is Ba 0.796Al 11.755Mn 0.237B 0.006O 18.670
Its chemical formula by analysis of embodiment 9 is Ba 0.797Al 11.758Mn 0.238B 0.008O 18.678
Its chemical formula by analysis of embodiment 10 is Ba 0.798Al 11.757Mn 0.236B 0.006O 18.672
Its chemical formula by analysis of embodiment 11 is Ba 0.795Al 11.753Mn 0.235B 0.006O 18.664
[add 0.01 mole bariumchloride or aluminum trifluoride or aluminum trifluoride or barium fluoride (BaF in the fluorescent material of every mole of embodiment 8-11 respectively by taking by weighing raw material and additive shown in the table 3 2)+aluminum fluoride (AlF 3), BaF 2With AlF 3Mol ratio be 1: 1], all the other conditions are with embodiment 1.Gained fluorescent material intensity is listed in the table 3.During with different additive, the luminous intensity of embodiment 8-11 all is higher than comparing embodiment.
The raw material of table 3 embodiment 8-11, additive and luminous intensity embodiment raw material (mole) additive luminous intensity (%)
BaCO 3Al 2O 3MnCO 3H 3BO 3(mole) 8 0.80 5.875 0.24 0.01 BaCl 20.01 114 9 0.80 5.875 0.24 0.01 AlCl 30.01 112 10 0.80 5.875 0.24 0.01 AlF 30.01 113 11 0.80 5.875 0.24 0.01 BaF 2+ AlF 3114
0.01
BaF 2∶AlF 3
Mol ratio 1: 1
Embodiment 12
Its chemical formula is Ba by analysis 0.698Al 11.852Mn 0.135B 0.003O 18.82, its working method is with embodiment 1.The additive barium fluoride is 0.003 mole, obtains result similar to Example 1.
Embodiment 13
Its chemical formula is Ba by analysis 0.877Al 11.770Mn 0.132B 0.089O 18.90, its working method is with embodiment 1.The additive barium fluoride is 0.085 mole, obtains result similar to Example 2.

Claims (12)

1. the aluminate green fluorescent powder of an excited by vacuum ultraviolet is characterized in that, the chemical formula of this green emitting phosphor is BaxAl 12-y-zMnyBzO 19, 0.699≤x≤0.99,0.13≤y≤0.3,0.001≤z≤0.1 wherein.
2. the manufacture method of the aluminate green fluorescent powder of an excited by vacuum ultraviolet is characterized in that,
1) presses chemical formula BaxAl 12-y-zMnyBzO 190.699≤x≤0.99 wherein, 0.13≤y≤0.3,0.001 prepare burden in≤z≤0.1, with wherein a kind of of barium oxide, barium salt is the raw material of barium, is the raw material of aluminium with wherein a kind of of aluminum oxide, hydrogen aluminum hydride, Burow Solution, is the raw material of manganese with wherein a kind of of Manganse Dioxide, manganese salt, with boron trioxide or boric acid is the raw material of boron
2) add additive in batching, the amount of additive is to add 0.001～0.1 mole alkaline earth metal halide or the halogenide of aluminium or the halid mixture of alkaline earth metal halide and aluminium in every mole of fluorescent material,
3) will grind the even compound that forms that is mixed as the raw material of barium, the raw material of aluminium, the raw material of manganese, the raw material and the additive of boron,
4) under the reductive condition in 1300-1450 ℃ with compound calcination 2-10 hour, form firing product,
5) product of calcination is added water and carry out ball milling and form the powder slurry, wash, filter the back oven dry with hot water.
3. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that said additive alkaline earth metal halide is wherein a kind of of barium fluoride, bariumchloride; The halogenide of additive-aluminium is wherein a kind of of aluminum chloride, aluminum fluoride, and the mixture of halides of additive alkaline earth metal halide and aluminium is 1: 1 the mixture of mol ratio of barium fluoride and aluminum fluoride.
4. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that said barium salt is barium oxalate, barium carbonate, barium acetate a kind of barium salt wherein.
5. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that said manganese salt is manganous carbonate, manganous oxalate, manganous sulfate a kind of manganese salt wherein.
6. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that, will as the raw material of the raw material of the raw material of the raw material of barium, aluminium, manganese, boron and additive be dry grinded or water mill 4-15 hour, the mill even compound that forms that is mixed.
7. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 1 or 6, it is characterized in that the weight ratio of ball and all raw materials and additive total amount was 1: 0.5～1.5 when mill mixed.
8. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that said reductive condition is for to carry out high temperature sintering in the atmosphere of hydrogen or nitrogen and hydrogen gas mixture.
9. the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet according to Claim 8 is characterized in that, the volume ratio of nitrogen and hydrogen is 1: 0.04～4 in the mixed gas of nitrogen and hydrogen.
10. according to the manufacture method of the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 2, it is characterized in that, after firing product adds entry, carried out ball milling 1-5 hour, form the powder slurry.
11. the manufacture method according to the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 10 is characterized in that, the water yield that is added is a firing product and the weight ratio of the water that is added is 1: 0.5～2.5.
12. the manufacture method according to the aluminate green fluorescent powder of a kind of excited by vacuum ultraviolet of claim 10 is characterized in that the weight ratio of ball and firing product is 1: 0.5～1.5 during ball milling.
CN 01110746 2001-04-19 2001-04-19 Vacuum ultraviolet excited green aluminate fluorescent powder and its preparing process Expired - Lifetime CN1219848C (en)

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Cited By (2)

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CN101372616B (en) * 2007-08-24 2011-11-09 北京有色金属研究总院 Vacuum ultraviolet excitated high color domain coverage ratio green phosphor and producing method thereof
CN104419424A (en) * 2013-08-19 2015-03-18 吴振华 LED yellow phosphor and production method thereof

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CN101130691B (en) * 2007-08-03 2010-06-09 西安理工大学 Method for improving luminous intensity of vacuum ultraviolet luminescent material with beta-Al2O3 structure
CN105001860B (en) * 2015-08-11 2018-12-18 王海容 A kind of red-emitting phosphors and its application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101372616B (en) * 2007-08-24 2011-11-09 北京有色金属研究总院 Vacuum ultraviolet excitated high color domain coverage ratio green phosphor and producing method thereof
CN104419424A (en) * 2013-08-19 2015-03-18 吴振华 LED yellow phosphor and production method thereof

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