CN100412158C - White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device - Google Patents
White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device Download PDFInfo
- Publication number
- CN100412158C CN100412158C CNB2004100417849A CN200410041784A CN100412158C CN 100412158 C CN100412158 C CN 100412158C CN B2004100417849 A CNB2004100417849 A CN B2004100417849A CN 200410041784 A CN200410041784 A CN 200410041784A CN 100412158 C CN100412158 C CN 100412158C
- Authority
- CN
- China
- Prior art keywords
- manufacturing process
- fluorescent powder
- blue
- process according
- light excited
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 title claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000000889 atomisation Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 5
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 5
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 5
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 27
- 239000003595 mist Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 229920000742 Cotton Polymers 0.000 claims description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000011449 brick Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract 1
- 238000009423 ventilation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 239000007787 solid Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 238000010574 gas phase reaction Methods 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses white light fluorescent powder excited by blue light, and application, a manufacturing process and a device thereof. The molecular formula of the fluorescent powder is aY2O3·bGd2O3·(1.5-a-b)Re2O3·2.5Al2O3·xSiO2Wherein: re is one or more of Ce, Eu, Tm and Tb; a is more than or equal to 1.02 and less than 1.5, b is more than or equal to 0 and less than 1.5, and x is more than 0 and less than 3; the fluorescent powder can be used for manufacturing white light LEDs. The process comprises the steps of precursor solution preparation, ventilation, atomization, reaction, collection and post-treatment. The device comprises a liquid adding device, an atomization generating device, a gas supply device, a gas flow control device, a reaction furnace, a powder collecting device and a purification treatment device. The invention has simple process, high efficiency and manufactured fluorescenceThe powder has good quality and is suitable for industrial large-scale production; the manufacturing equipment has low cost and high efficiency.
Description
Technical field
The present invention relates to a kind of fluorescent material, particularly relate to a kind of blue-light excited white emitting fluorescent powder, the invention still further relates to its purposes, manufacturing process and manufacturing installation.
Background technology
Yttrium aluminum garnet Y
3Al
5O
12(being called for short YAG) has good thermal conductivity and physical strength and good physicochemical property.Be widely used as laser and luminous substrate material.Ce
3+The activated yttrium aluminium garnet YAG: the Ce excitation wavelength can absorb the blue light that GaN sends effectively near 460nm.The emission wavelength of YAG:Ce can constitute high-brightness white-light with the blue light of LED is compound about 540nm, can obtain the white light source that luminous efficiency is high and be suitable for throwing light on.The energy consumption of this class LED (photodiode) white light pipe is about 20% of a head light commonly used, is rising energy-conserving light source.The traditional synthetic method of this class material is again through ball mill pulverizing behind the employing high temperature solid state reaction, its drawback is that synthesis temperature is too high, the product particle diameter is bigger than normal and size-grade distribution is wide, be difficult to the granularity that reaches satisfied, and the utmost point is difficult to obtain monophasic cube of garnet structure.
Prepare the softening length of schooling Preparation Methods such as sol-gel method, coprecipitation method, hydrothermal method in addition of YAG fluorescent material at present both at home and abroad, though can obtain the powder of better performances, be easy to generate reunion, cost is higher, is not suitable for shortcomings such as scale operation.
Summary of the invention
The purpose of this invention is to provide between a kind of particle and to form the blue-light excited white emitting fluorescent powder that identical, particle mostly is spherical, good fluidity, powder tap density height, luminosity height, is fit to industrial mass production.
Another object of the present invention provides the purposes of above-mentioned fluorescent material.
A further object of the invention provides the manufacturing process of above-mentioned fluorescent material.
A further object of the invention provides the device of above-mentioned fluorescent material manufacturing process.
Technical scheme of the present invention be form vapor phase solvent according to atomizing droplet size relatively evenly, have large surface area to react, principle that reaction efficiency is high, design a kind of technology of gas-phase reaction manufactured fluorescent material, utilize a kind of gas-phase reaction device to synthesize blue-light excited white emitting fluorescent powder, solid sphere, narrow diameter distribution, brightness height, tap density that institute's synthetic fluorescent material is rule are big, can be applicable to white light LEDs aspects such as (photodiodes).
The objective of the invention is to realize by following measures:
A kind of blue-light excited white emitting fluorescent powder, its molecular formula can be written as:
aY
2O
3·bGd
2O
3·(1.5-a-b)Re
2O
3·2.5Al
2O
3·xSiO
2
Wherein:
Re is Ce, Eu, Tm, one or more among the Tb;
1.02≤a＜1.5，0≤b＜1.5，0＜x＜3。
Described blue-light excited white emitting fluorescent powder manufacturing process, this technology may further comprise the steps:
(1) takes by weighing by corresponding cationic stoichiometric ratio in the fluorescent material and contain corresponding cationic soluble compound dissolving and be mixed with certain density precursor solution, in the mist generating device of packing into;
(2) feed inertia or reducing gas or oxidizing gas in reactive system, the gas flow of maintenance is at 1-100L/min;
(3) start atomisation unit, precursor solution begins to be atomized into mist, crosses reaction chamber with air flow stream, and reaction generates the presoma or the finished product of fluorescent material under 500-1800 ℃ of temperature, collects;
(4) presoma or the finished product of collecting can be obtained satisfactory fluorescent material through aftertreatment.
Described manufacturing process, wherein said soluble compound are to contain in Nitrates, Sulfates, chloride-based and the organic salt thereof of Y, Gd, Al, Si, Ce, Eu, Tm, Tb element or one or more of other soluble compound.
Described manufacturing process wherein also can add certain quantity of additive in the precursor solution, and additive is a polyoxyethylene glycol, and add-on is that every ml soln adds the 0-1g additive.
Described manufacturing process, wherein in the precursor solution cationic concentration range at 0.01-4.0mol/L.
Described manufacturing process, wherein collected diameter of particle is along with the increase of the cation concn of precursor solution increases to 8.0 μ m by 0.1 μ m.
Described manufacturing process, gas wherein comprises N
2, Ar, He, Ne, CO, H
2, O
2, airborne one or more.
Described manufacturing process, wherein aftertreatment comprises: at 900-1800 ℃, calcination 0.5-5h under the reducing atmosphere also comprises and fluorescent material is washed for several times dewatered drying in deionized water or in the weak acid.
Described manufacturing process, wherein weak acid can be mineral acid or organic acid, pH value scope is at 3-7.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, this covering device comprises liquid-adding device, mist generating device, gas supply device, gas flow control device, Reaktionsofen, powder collection device, purifying processing device.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, wherein the gas supply device air outlet is being connected with the supersonic atomizer inlet mouth through behind the gas flow control device, the liquid-adding device liquid outlet is connected with the mist generating device fluid inlet, controls liquid feeding by the fluid level control device of atomisation unit inside; The outlet of atomisation unit is connected with the opening for feed of Reaktionsofen, and the discharge port of Reaktionsofen is connected with the powder collection device, and the gas that comes out from the powder collection device passes through to arrange to atmosphere behind the purifying processing device.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, wherein mist generating device can be a supersonic atomizer; Supersonic atomizer is made up of container, ultrasonic atomization wafer, PCB (printed circuit board (PCB)) Controlling System, fluid level control device.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, wherein Reaktionsofen can be a tubular react furnace; Tubular react furnace includes crystal reaction tube, cylinder bodily form burner hearth, and hearth outer wall twines the resistance heating wire, and light fire brick, insulating cotton have also been built in the outside, and temperature of reaction is between 200-1500 ℃; This tubular react furnace is many warm area controls, includes 1-40 independent heating warm area, and each warm area is furnished with a point for measuring temperature.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, wherein collection device is a kind of in folded filter paper formula collection device, filter bag type collection device, tornado collection device, the electrostatic collection device.
The device of described blue-light excited white emitting fluorescent powder manufacturing process, wherein the angle of Reaktionsofen and horizontal plane is adjustable in 0-180 °, the length 0.5-30m of Reaktionsofen.
The described blue-light excited application of white emitting fluorescent powder in LED (photodiode).
Advantage of the present invention:
The fluorescent material of the present invention's preparation can send white light under blue-light excited, be particularly useful for white light LEDs (photodiode) manufacturing; Manufacturing process adopts gas-phase reaction method technology simple, and solute is separated out at short notice, and composition is identical between the fluorescent powder grain of manufacturing, and it is spherical that particle mostly is, good fluidity, and powder tap density height, the brightness height is fit to advantages such as industrial mass production; The producing apparatus cost is low, efficient is high.
Description of drawings
Fig. 1 is that gas-phase reaction method prepares fluorescent material equipment synoptic diagram.
Embodiment
The invention will be further elaborated by following examples in conjunction with Figure of description.
Embodiment 1:
Take by weighing Y
2O
328.2404g, Gd
2O
3Become the clarification rare earth nitrate aqueous solution 8.1947g be dissolved in an amount of nitric acid, add Al (NO again
3)
39H
2O 189.4611g, H
2SiO
33.9050g, Ce (NO
3)
36H
2O2.5502g adds deionized water dilution 2000ml, and this mixing solutions is the precursor solution of reaction to be atomized, and solution is added automatic liquid feeder 1.Many warm areas tubular react furnace 6 is warming up to 1300 ℃, and temperature is by temperature control system 7 controls.Tubular react furnace includes crystal reaction tube, cylinder bodily form burner hearth, hearth outer wall twines the resistance heating wire, also build the outside light fire brick, insulating cotton, this tubular react furnace is many warm area controls, include 4 independent heating warm areas, each warm area is furnished with a point for measuring temperature, and Reaktionsofen keeps level, and the length of Reaktionsofen is 2m.Open valve 2 injects supersonic atomizer 3 to certain liquid level with precursor solution, supersonic atomizer is made up of container, ultrasonic atomization wafer, PCB Controlling System, fluid level control device, ultrasonic atomization wafer number is 10, and operating frequency is 1.7 ± 0.1MHz.With N in the gas supply device 4
2The feeding system in, make the air emptying in supersonic atomizer 3, many warm areas tubular react furnace 6, the tornado collection device 8, keep N by gas flow control device 5
2Flow at 20L/min.Open supersonic atomizer 3, precursor solution begins to be atomized into mist, and with the too much warm area tubular react furnace 6 of air communication, the fluorescent material that reaction obtains is collected by tornado collection device 8 and entered in the container 10, and residual air then purifies the back by purifying processing device 9 and discharges.Fluorescent material deionized water wash 3 times with collecting promptly obtain consisting of 1.245Y behind dewatered drying
2O
30.225Gd
2O
32.5Al
2O
30.03CeO
20.5SiO
2Finished product.With its pattern of scanning electron microscopic observation, be solid sphere, D
50Be 2 μ m, its size distribution is better than comparative example, and its brightness the results are shown in Table 1 apparently higher than comparative example.
Implement comparative example: take by weighing Y
2O
328.2404g, Al
2O
325.4928g, SiO
23.0045g, Gd
2O
38.1947g, CeO
21.0396g add an amount of solubility promoter ball milling,, and, obtain consisting of 1.245Y through dewatered drying with deionized water wash 3 times in the calcining two hours down of 1600 ℃ of reducing atmospheres
2O
30.225Gd
2O
32.5Al
2O
30.03CeO
20.5SiO
2Fluorescent material.
Each material purity is: Y
2O
3: 99.56%; Gd
2O
3: 99.54%; Al (NO
3)
39H
2O＞99%; Ce (NO3)
36H
2O:CeO
2: 40.5%; Al
2O
3: 99.99%; SiO
2:: 99.99%.
Table 1 gas-phase reaction method and solid reaction process synthetic product are relatively
(1.245Y
2O
3·0.225Gd
2O
3·2.5Al
2O
3·0.03CeO
2·0.5SiO
2)
| Classification | Solid phase method is synthetic | Vapor phase process is synthetic |
| Relative brightness (%) | 100 | 124 |
| Emission main peak (nm) | 541 | 538 |
| Size distribution | Wide | Narrow |
| Pattern | Irregular | Solid sphere |
| Dispersed | Reunite and lump, need ball milling | Be uniformly dispersed |
Take by weighing Y
2O
3231.3673g, Gd
2O
3Become the clarification rare earth nitrate aqueous solution 163.8944g be dissolved in an amount of nitric acid, add Al (NO again
3)
39H
2O 1894.6110g, H
2SiO
339.0500g, Ce (NO
3)
36H
2O25.5020g adds deionized water dilution 5000ml, and this mixing solutions is the precursor solution of reaction to be atomized, and solution is added automatic liquid feeder 1.Many warm areas tubular react furnace 6 is warming up to 800 ℃, and temperature is by temperature control system 7 controls.Tubular react furnace includes crystal reaction tube, cylinder bodily form burner hearth, hearth outer wall twines the resistance heating wire, also build the outside light fire brick, insulating cotton, this tubular react furnace is many warm area controls, include 10 independent heating warm areas, each warm area is furnished with a point for measuring temperature, and the angle of Reaktionsofen and horizontal plane is 15 °, and the length of Reaktionsofen is 5m.Open valve 2 injects supersonic atomizer 3 to certain liquid level with precursor solution, supersonic atomizer is made up of container, ultrasonic atomization wafer, PCB Controlling System, fluid level control device, ultrasonic atomization wafer number is 30, and operating frequency is 1.7 ± 0.1MHz.In the feeding system with He in the gas supply device 4, make the air emptying in supersonic atomizer 3, many warm areas tubular react furnace 6, the filter bag collection device 8, keep N by gas flow control device 5
2Flow at 70L/min.Open supersonic atomizer 3, precursor solution begins to be atomized into mist, and with the too much warm area tubular react furnace 6 of air communication, the fluorescent material that reaction obtains is collected by filter bag collection device 8 and entered in the container 10, and residual air then purifies the back by purifying processing device 9 and discharges.With the fluorescent material collected calcination 1h under 1500 ℃, reducing atmosphere, be washing 2 times in rare nitric acid of 3 in the pH value, again with deionized water wash once, dewatered drying promptly gets and consists of 1.02Y
2O
30.45Gd
2O
32.5Al
2O
30.03CeO
20.5SiO
2Finished product.With its pattern of scanning electron microscopic observation, be solid sphere, D
50Be 5 μ m, its size distribution is better than comparative example, and its brightness the results are shown in Table 2 apparently higher than comparative example.
Implement comparative example: take by weighing Y
2O
3231.3673g, Al
2O
3254.9280g, SiO
230.0450g, Gd
2O
3163.8944g, CeO
210.396g add an amount of solubility promoter ball milling, in the calcining two hours down of 1600 ℃ of reducing atmospheres, in being rare nitric acid of 3, pH value washs 2 times, more once, obtain consisting of 1.02Y through dewatered drying with deionized water wash
2O
30.45Gd
2O
32.5Al
2O
30.03CeO
20.5SiO
2Fluorescent material.
Each material purity is: Y
2O
3: 99.56%; Gd
2O
3: 99.54%; Al (NO
3)
39H
2O＞99%; Ce (NO3)
36H
2O:CeO
2: 40.5%; Al
2O
3: 99.99%; SiO
2:: 99.99%.
Table 2 gas-phase reaction method and solid reaction process synthetic product are relatively
(1.02Y
2O
3·0.45Gd
2O
3·2.5Al
2O
3·0.03CeO
2·0.5SiO
2)
| Classification | Solid phase method is synthetic | Vapor phase process is synthetic |
| Relative brightness (%) | 100 | 129 |
| Emission main peak (nm) | 551 | 557 |
| Size distribution | Wide | Narrow |
| Pattern | Irregular | Solid sphere |
| Dispersed | Reunite and lump, need ball milling | Be uniformly dispersed |
Claims (14)
1. blue-light excited white emitting fluorescent powder, its molecular formula can be written as:
aY
2O
3·bGd
2O
3·(1.5-a-b)Re
2O
3·2.5Al
2O
3·xSiO
2
Wherein:
Re is Ce, Eu, Tm, one or more among the Tb;
1.02≤a＜1.5，0≤b＜1.5，0＜x＜3。
2. blue-light excited white emitting fluorescent powder manufacturing process as claimed in claim 1, this technology may further comprise the steps:
(1) takes by weighing by corresponding cationic stoichiometric ratio in the fluorescent material and contain corresponding cationic soluble compound dissolving and be mixed with certain density precursor solution, in the mist generating device of packing into;
(2) feed inertia or reducing gas or oxidizing gas in reactive system, the gas flow of maintenance is at 1-100L/min;
(3) start atomisation unit, precursor solution begins to be atomized into mist, crosses reaction chamber with air flow stream, and reaction generates the presoma or the finished product of fluorescent material under 500-1800 ℃ of temperature, collects;
(4) presoma or the finished product of collecting can be obtained satisfactory fluorescent material through aftertreatment.
3. manufacturing process according to claim 2 is characterized in that described compound is to contain in Nitrates, Sulfates, chloride-based and the organic salt thereof of Y, Gd, Al, Si, Ce, Eu, Tm, Tb element one or more.
4. manufacturing process according to claim 2 is characterized in that also can adding certain quantity of additive in the precursor solution, and additive is a polyoxyethylene glycol, and add-on is that every ml soln adds the 0-1g additive.
5. manufacturing process according to claim 2 is characterized in that cationic concentration range is at 0.01-4.0mol/L in the precursor solution.
6. manufacturing process according to claim 2 is characterized in that collected diameter of particle is along with the increase of the cation concn of precursor solution increases to 8.0 μ m by 0.1 μ m.
7. manufacturing process according to claim 2 is characterized in that described gas comprises N
2, Ar, He, Ne, CO, H
2, O
2, airborne one or more.
8. manufacturing process according to claim 2, it is characterized in that described aftertreatment comprises: at 900-1800 ℃, calcination 0.5-5h under the reducing atmosphere, also comprise fluorescent material is washed in deionized water or in the weak acid for several times, weak acid can be mineral acid or organic acid, pH value scope is at 3-7, dewatered drying.
9. the device of the described blue-light excited white emitting fluorescent powder manufacturing process of claim 2 is characterized in that this covering device comprises liquid-adding device, mist generating device, gas supply device, gas flow control device, Reaktionsofen, powder collection device, purifying processing device; Wherein the gas supply device air outlet is being connected with the supersonic atomizer inlet mouth through behind the gas flow control device, and the liquid-adding device liquid outlet is connected with the mist generating device fluid inlet, controls liquid feeding by the fluid level control device of atomisation unit inside; The outlet of atomisation unit is connected with the opening for feed of Reaktionsofen, and the discharge port of Reaktionsofen is connected with the powder collection device, and the gas that comes out from the powder collection device passes through to arrange to atmosphere behind the purifying processing device.
10. the device of blue-light excited white emitting fluorescent powder manufacturing process according to claim 9 is characterized in that described mist generating device can be a supersonic atomizer; Supersonic atomizer is made up of container, ultrasonic atomization wafer, plated circuit Controlling System, fluid level control device.
11. the device of blue-light excited white emitting fluorescent powder manufacturing process according to claim 9 is characterized in that described Reaktionsofen can be a tubular react furnace; Tubular react furnace includes crystal reaction tube, cylinder bodily form burner hearth, and hearth outer wall twines the resistance heating wire, and light fire brick, insulating cotton have also been built in the outside, and temperature of reaction is between 200-1800 ℃; This tubular react furnace is many warm area controls, includes 1-40 independent heating warm area, and each warm area is furnished with a point for measuring temperature.
12. the device of blue-light excited white emitting fluorescent powder manufacturing process according to claim 9 is characterized in that described collection device is a kind of in folded filter paper formula collection device, filter bag type collection device, tornado collection device, the electrostatic collection device.
13. the device according to claim 9 or 11 described blue-light excited white emitting fluorescent powder manufacturing process is characterized in that the angle of described Reaktionsofen and horizontal plane is adjustable in 0-180 °, the length 0.5-30m of Reaktionsofen.
14. the described blue-light excited application of white emitting fluorescent powder in LED of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100417849A CN100412158C (en) | 2004-08-25 | 2004-08-25 | White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100417849A CN100412158C (en) | 2004-08-25 | 2004-08-25 | White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1597841A CN1597841A (en) | 2005-03-23 |
| CN100412158C true CN100412158C (en) | 2008-08-20 |
Family
ID=34665254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100417849A Expired - Fee Related CN100412158C (en) | 2004-08-25 | 2004-08-25 | White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100412158C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312252C (en) * | 2005-11-28 | 2007-04-25 | 广州有色金属研究院 | Method and apparatus for preparing PDP fluorescent material |
| KR100939936B1 (en) * | 2006-06-21 | 2010-02-04 | 대주전자재료 주식회사 | Thullium Containing Fluorescent Substance For White Light Emitting Diode And Manufacturing Method Thereof |
| CN101210181B (en) * | 2006-12-29 | 2010-05-19 | 财团法人工业技术研究院 | Fluorescent material, white light luminescent device and false proof coating |
| CN101126024B (en) * | 2007-09-07 | 2010-06-09 | 江苏博睿光电有限公司 | Fluorescent powder for white light emitting diode and preparation method thereof |
| CN101705095B (en) * | 2009-09-21 | 2011-08-10 | 四川新力光源有限公司 | Yellow light afterglow material and preparation method thereof as well as LED illuminating device using same |
| CN103217016B (en) * | 2013-04-09 | 2015-10-07 | 南京信息职业技术学院 | Inorganic powder material synthesizer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5104573A (en) * | 1988-10-17 | 1992-04-14 | Sony Corporation | Green light emitting phosphor |
| CN1331272A (en) * | 2000-06-26 | 2002-01-16 | 中国科学院长春光学精密机械与物理研究所 | Wavelength-converting luminous material of white light for LED |
| US20020013215A1 (en) * | 2000-04-06 | 2002-01-31 | Ryouhei Nakamura | Ceramics and their powder for scintillators, and method for producing same |
| CN1362465A (en) * | 2000-12-30 | 2002-08-07 | 大连路明发光科技股份有限公司 | New type long-persistence material |
-
2004
- 2004-08-25 CN CNB2004100417849A patent/CN100412158C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5104573A (en) * | 1988-10-17 | 1992-04-14 | Sony Corporation | Green light emitting phosphor |
| US20020013215A1 (en) * | 2000-04-06 | 2002-01-31 | Ryouhei Nakamura | Ceramics and their powder for scintillators, and method for producing same |
| CN1331272A (en) * | 2000-06-26 | 2002-01-16 | 中国科学院长春光学精密机械与物理研究所 | Wavelength-converting luminous material of white light for LED |
| CN1362465A (en) * | 2000-12-30 | 2002-08-07 | 大连路明发光科技股份有限公司 | New type long-persistence material |
Non-Patent Citations (2)
| Title |
|---|
| 白光 LED现状和问题. 刘行仁等.中国照明电器，第3期. 2003 |
| 白光 LED现状和问题. 刘行仁等.中国照明电器，第3期. 2003 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1597841A (en) | 2005-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101602944B (en) | Method for producing rare earth ion doped yttrium aluminum garnet nano phosphor powder | |
| KR100681110B1 (en) | Method and apparatus for preparing luminescent material with high brightness | |
| CN100412158C (en) | White light fluorescent powder excited by blue light and its use, manufacturing process and manufacturing device | |
| CN103864143B (en) | The preparation method of nano zircite pelletizing | |
| CN101760196A (en) | Method for combining yellow fluorescent powder used for white light LED | |
| CN207347181U (en) | Rafifinal atomization explosion method prepares the device of high-purity alumina powder | |
| JPH02501477A (en) | Method for producing metal oxide powder | |
| CN100339460C (en) | Preparation method of silicate luminous body for converting blue light to white light | |
| CN209060564U (en) | A kind of spray drying production equipment of low-temperature SCR catalyst powder | |
| CN103303961B (en) | Preparation method of spherical electroplating-level copper oxide powder | |
| CN108017388B (en) | Lanthanum zirconate-based ceramic granulation powder for atmospheric plasma spraying and preparation method thereof | |
| CN107163942A (en) | Small particle cerium dropped yttrium aluminum garnet fluorescent material and method and application prepared by a kind of coprecipitation | |
| CN208860113U (en) | A kind of rotary kiln material collecting device | |
| CN101182415A (en) | Yellow fluorescent powder and method for making same | |
| JP2010208917A (en) | Method and device for pulse spray thermal decomposition | |
| CN201031206Y (en) | Aerosol atomising device | |
| CN100564479C (en) | Red fluorescent powder and preparation process thereof | |
| CN100441658C (en) | Method of preparing yttrium aluminium garnet fluorescent powder | |
| CN116285437A (en) | Preparation method of aerosol spray-coated nano bismuth-europium co-doped yttrium oxide fluorescent powder coating | |
| CN1244534C (en) | Technological process for producing sodium oxalate by liquid-spraying type sodium formate dehydrogenation and use equipment | |
| CN100345937C (en) | White-light diode silicate single-substrate fluorescent body and its preparing method | |
| CN104211107B (en) | The preparation method of nano tin-oxide powder | |
| CN100334185C (en) | Rare-earth yttrium-aluminium garnet luminous material and its gas-phase preparing method | |
| CN100556984C (en) | Shell-grade red illuminating material for lamp and preparation method thereof | |
| CN2257496Y (en) | Spray pyrolytic device for preparing hollow tiny powder material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Jiangsu Yong Shi Lighting Co.,Ltd. Assignor: Nanjing Tech University Contract fulfillment period: 2009.8.31 to 2012.8.30 Contract record no.: 2009320001624 Denomination of invention: White light fluorescence powder excitated by blue light and its application mfg. technology and mfg. apparatus Granted publication date: 20080820 License type: Exclusive license Record date: 20090902 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.8.31 TO 2012.8.30; CHANGE OF CONTRACT Name of requester: JIANGSU YONGSHI LIGHTING CO., LTD. Effective date: 20090902 |
|
| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: JIANGSU YONG SHI LIGHTING Co.,Ltd. Assignor: Nanjing Tech University Contract record no.: 2009320001624 Date of cancellation: 20140923 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20050323 Assignee: JIANGSU HAODE ENERGY-SAVING PHOTOELECTRICITY TECHNOLOGY CO.,LTD. Assignor: Nanjing Tech University Contract record no.: 2015320000144 Denomination of invention: White light fluorescence powder excitated by blue light and its application mfg. technology and mfg. apparatus Granted publication date: 20080820 License type: Common License Record date: 20150407 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080820 Termination date: 20170825 |