CN100506946C - Preparation method of aluminate base blue color fluorescent powder - Google Patents
Preparation method of aluminate base blue color fluorescent powder Download PDFInfo
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- CN100506946C CN100506946C CNB2006101093687A CN200610109368A CN100506946C CN 100506946 C CN100506946 C CN 100506946C CN B2006101093687 A CNB2006101093687 A CN B2006101093687A CN 200610109368 A CN200610109368 A CN 200610109368A CN 100506946 C CN100506946 C CN 100506946C
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- 239000000843 powder Substances 0.000 title claims abstract description 86
- 150000004645 aluminates Chemical class 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 239000000725 suspension Substances 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 230000018044 dehydration Effects 0.000 claims abstract description 9
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000011777 magnesium Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910021645 metal ion Inorganic materials 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910001422 barium ion Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000002572 peristaltic effect Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 abstract description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Inorganic materials [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- 238000005303 weighing Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 229910020068 MgAl Inorganic materials 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 159000000009 barium salts Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910015999 BaAl Inorganic materials 0.000 description 1
- 241000282693 Cercopithecidae Species 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000003407 synthetizing effect Effects 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
Abstract
The present invention relates to a preparation method of aluminate base blue fluorescent powder. It is characterized by that said preparation method includes the following steps: using Ba(NO3)2 and Mg (NO3)2.6H2O to prepare solution, adding Eu(NO3)2 into the above-mentioned solution, then adding suspension of spherical basic ammonium aluminium carbonate, stirring them to make reaction, standing still to make precipitation, washing, dehydration, drying to obtain bulky powder body, drying said powder body and calcining so as to obtain blue fluorescent powder.
Description
Technical field
A kind of preparation method of aluminate blue fluorescent powder relates to a kind of employing heterogeneous precipitation method and prepares the aluminate blue fluorescent powder commercial run.
Background technology
For a long time, industrial synthetic BAM blue colour fluorescent powder mainly adopts traditional high temperature solid-state method, as the method for preparing aluminate blue fluorescent powder among Chinese patent CN1415695A, the CN1673314A is with raw material and an amount of fusing assistant mixing such as aluminum oxide, barium oxide, magnesium oxide, europium sesquioxides, calcination under 1400～1700 ℃ the temperature in reducing atmosphere is then then carried out firing product Ball milling, washing, drying, is sieved.Though this method technology is simple; easily accomplish scale production; but building-up process generally needs long high temperature sintering; though the adding of fusing assistants such as boric acid can make synthesis temperature significantly reduce; but also make the serious sintering of fluorescent material; and solid phase method synthetic fluorescent powder grain profile is irregular; powder body material is mobile poor; be unfavorable for being coated with screen; must reduce the fluorescent material particle diameter by methods such as Ball milling; thereby cause the fluorescent powder grain surface damage, destroyed the BAM structure, make the luminescent properties of fluorescent material sharply descend.Simultaneously, also often inhomogeneous in the production process because of the raw material mixing, cause reaction not exclusively to contain α-Al
2O
3, BaAl
2O
4, MgAl
2O
4Deng dephasign, these dephasigns easily absorb uv-radiation and visible light causes light decay.
For addressing this problem, people attempt other novel procesies and synthesize " non-ball millingization " high-performance BAM blue powder, adopt the Prepared by Sol Gel Method aluminate-base fluorescent powder as Chinese patent CN1334309A, metal ion and citric acid solution reaction are formed colloidal sol, gel, through pre-burning, sieve, calcination under reducing atmosphere at last, obtain the fluorescent material of granularity between 0.1～10 μ m, but this method process cycle is long, cost is high, and is difficult to prepare particle diameter less than 4 μ m and the aluminate fluorescent powder that is evenly distributed.In addition, Chinese patent CN1664057A adopts coprecipitation method to prepare aluminate-base fluorescent powder, bicarbonate of ammonia and additive mixing solutions with 20～80 ℃ of metallic ion mixed liquor addings, through dehydration, oven dry, calcination under 1000～1500 ℃ the temperature in reducing atmosphere then, at last firing product is washed, dry, sieve, but during this method synthetizing phosphor powder, the Al ion is easily with Al (OH)
3The gel form precipitation, and the precipitated product primary particle is minimum by (about 5～10nm), sintering and hard aggregation can take place when high temperature sintering, still there is thick, the serious problem of reuniting of particle in fluorescent material, be difficult to prepare real ball milling free aluminate fluorescent powder, and the particle profile that makes is hexagonal plate, and powder body material is mobile poor, is unfavorable for being coated with screen.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art and shortcoming, provide a kind of granularity of can preparing at 1～5 μ m, the particle profile is spherical in shape, promptly can be used as luminescent lamp, plasma display (PDP) or three primary colors fluorescent powder uses without ball milling, and the heterogeneous precipitation method with fluorescent material of higher photoluminescence efficiency prepares the processing method of aluminate blue fluorescent powder.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of aluminate base blue colour fluorescent powder is characterized in that preparation process comprises:
A. with Ba (NO
3)
2And Mg (NO
3)
26H
2O is mixed with settled solution with deionized water, gets solution A;
B. with Eu (NO
3)
3Solution adds to solution A, stirs, and it is mixed, and gets solution B;
C. spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the deionized water, gets suspension C;
D. in suspension C, add H then
2C
2O
42H
2O stirs, and makes it to dissolve fully, gets suspension D;
E. regulate the pH value of suspension D with NaOH solution, solution B is at the uniform velocity added stirring reaction among the suspension D, regulate control pH with NaOH solution; Behind the reinforced end of processing, behind the continuation stirring reaction, staticly settle, with the throw out deionized water wash, dehydration, oven dry obtains fluffy powder;
F. the powder roasting after will drying makes aluminate base blue colour fluorescent powder.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention is characterized in that spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the suspension that forms in the deionized water, and the system solid content is 20～100g/L; Add oxalic acid and sodium hydroxide as precipitation agent, stir, system pH is controlled between 8.5～11.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, it is characterized in that it being chemical constitution preparing metal ionic mixing solutions by the aluminate base blue colour fluorescent powder that will prepare, barium and magnesium raw material are with respect to aluminium excessive 1%～100%, take by weighing corresponding soluble barium salt of institute and magnesium salts respectively, be dissolved in the deionized water, wherein the concentration of barium and magnesium ion is 0.05～2mol/L.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, it is characterized in that the mixing solutions of metal ion is at the uniform velocity joined in the AACH powder suspension by peristaltic pump, feed rate is controlled at 5～20mL/min, stirs simultaneously, and the pH value of precipitation system is between 8.5～11.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, after the mixing solutions that it is characterized in that metal ion dropwised, precipitation system continued to stir 1～5 hour, then stopped to stir, and left standstill, suction filtration, washing, dehydration, oven dry, obtained fluffy powder.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, it is characterized in that dried powder roasting temperature of 1200 to 1500 ℃ in reducing atmosphere is promptly obtained required blue colour fluorescent powder after 1～6 hour, wherein reducing atmosphere is provided by the carbon dust burning, or uses nitrogen/hydrogen mixed gas.
The inventive method uses heterogeneous precipitation method to prepare aluminate blue fluorescent powder.The chemical expression of the aluminate blue fluorescent powder of preparation is: (Ba
1-xEu
x) MgAl
10O
17, 0.05≤x≤0.2 wherein.Under condition of the present invention, barium, magnesium ion are with the spherical AACH powder of the wrapped of oxalate or precipitation of hydroxide, and powder granule sintering can not take place when high-temperature roasting, also do not produce distortion, thereby avoided the hard aggregation phenomenon effectively.
Method of the present invention, preparation technology is simple, cost is low, the cycle is short, is easy to engineering and amplifies; The aluminate blue fluorescent powder particle of preparing is spherical in shape, medium particle diameter 1～5 μ m, and need not ball milling can use; The fluorescent material synthesis temperature obviously reduces than solid phase method, helps energy efficient; This fluorescent material advantages of good crystallization, luminescent properties is superior.
Description of drawings
Fig. 1 detects blue powder (Ba for embodiment's in F-4500 type spectrophotofluorometer
1-xEu
x) MgAl
10O
17(x=0.1) emmission spectrum, excitation wavelength is at 350nm.
Embodiment
A kind of preparation method of aluminate base blue colour fluorescent powder, preparation process comprises: a. is with Ba (NO
3)
2And Mg (NO
3)
26H
2O is mixed with settled solution with deionized water, gets solution A; B. with Eu (NO
3)
3Solution adds to solution A, stirs, and it is mixed, and gets solution B; C. spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the deionized water, gets suspension C; D. in suspension C, add H then
2C
2O
42H
2O stirs, and makes it to dissolve fully, gets suspension D; E. regulate the pH value of suspension D with NaOH solution, solution B is at the uniform velocity added stirring reaction among the suspension D, regulate control pH with NaOH solution; Behind the reinforced end of processing, behind the continuation stirring reaction, staticly settle, with the throw out deionized water wash, dehydration, oven dry obtains fluffy powder; F. the powder roasting after will drying makes aluminate base blue colour fluorescent powder.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention is characterized in that spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the suspension that forms in the deionized water, and the system solid content is 20～100g/L; Add oxalic acid and sodium hydroxide as precipitation agent, stir, system pH is controlled between 8.5～11.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, chemical constitution preparing metal ionic mixing solutions by the aluminate base blue colour fluorescent powder that will prepare, barium and magnesium raw material are with respect to aluminium excessive 1%～100%, take by weighing corresponding soluble barium salt of institute and magnesium salts respectively, be dissolved in the deionized water, wherein the concentration of barium and magnesium ion is 0.05～2mol/L.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, the mixing solutions of metal ion is at the uniform velocity joined in the AACH powder suspension by peristaltic pump, feed rate is controlled at 5～20mL/min, stirs simultaneously, and the pH value of precipitation system is between 8.5～11.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, after the mixing solutions of metal ion dropwised, precipitation system continue to stir 1～5 hour, then stopped to stir, and left standstill, suction filtration, washing, dehydration, oven dry, obtained fluffy powder.
The preparation method of a kind of aluminate base blue colour fluorescent powder of the present invention, dried powder roasting temperature of 1200 to 1500 ℃ in reducing atmosphere is promptly obtained required blue colour fluorescent powder after 1～6 hour, wherein reducing atmosphere is provided by the carbon dust burning, or uses nitrogen/hydrogen mixed gas.
Embodiment 1
This example is to wrap up spherical AACH powder preparing PDP or blue fluorescent powder for fluorescent lamp Ba with barium, magnesium non-homogeneous phase deposition
0.9Eu
0.1MgAl
10O
17
Take by weighing 10.3225 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O is mixed with settled solution with deionized water, gets solution A, measures 36.5mL Eu (NO in addition
3)
3Solution (concentration 0.1M) adds to solution A, stirs, and it is mixed, and gets solution B; Take by weighing the spherical AACH powder of 50 grams and be scattered in the 2.5L deionized water, get suspension C, add 9.9595 gram H then
2C
2O
42H
2O stirs, and makes it to dissolve fully, gets suspension D, regulates pH=9.7 with NaOH solution; Solution B is at the uniform velocity added stirring reaction among the suspension D, regulate and control pH=9.7 with NaOH solution; Continue to stir 3 hours behind the reinforced end of processing; Stop to stir, staticly settle, outwell supernatant, with throw out deionized water wash 3 times, dehydration, oven dry obtains fluffy powder; Dried powder is packed in the less alumina crucible, uncoveredly do not add a cover, then it is placed in the bigger alumina crucible, between big crucible and monkey, put into carbon dust (as gac), big crucible cover top cover labyrinth, 1400 ℃ roasting temperatures got final product in 3 hours required blue colour fluorescent powder.In F-4500 type spectrophotofluorometer, detect blue powder (Ba
1-xEu
x) MgAl
10O
17(x=0.1) emmission spectrum, excitation wavelength is at 350nm.
Embodiment 2
Take by weighing 10.3225 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O, 36.5mL Eu (NO
3)
3Solution (0.1M concentration), 9.9595 gram H
2C
2O
42H
2O, the spherical AACH powder of 50 grams is regulated pH=8.5 with NaOH solution during precipitin reaction, and all the other are with embodiment 1.
Embodiment 3
Take by weighing 10.3225 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O, 36.5mL Eu (NO
3)
3Solution (0.1M concentration), 9.9595 gram H
2C
2O
42H
2O, the spherical AACH powder of 50 grams is regulated pH=11 with NaOH solution during precipitin reaction, and all the other are with embodiment 1.
Embodiment 4
Take by weighing 10.8960 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O, 19mL Eu (NO
3)
3Solution (0.1M concentration), 9.9595 gram H
2C
2O
42H
2O, the spherical AACH powder of 50 grams, all the other are with embodiment 1.
Embodiment 5
Take by weighing 9.1756 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O, 73mL Eu (NO
3)
3Solution (0.1M concentration), 9.9595 gram H
2C
2O
42H
2O, the spherical AACH powder of 50 grams, all the other are with embodiment 1.
Embodiment 6
Take by weighing 20.6450 gram Ba (NO
3)
2, 25.8092 gram Mg (NO
3)
26H
2O, 73mLEu (NO
3)
3Solution (0.1M concentration), 19.9190 gram H
2C
2O
42H
2O, the spherical AACH powder of 100 grams, all the other are with embodiment 1.
Embodiment 7
Take by weighing 22.5218 gram Ba (NO
3)
2, 25.8092 gram Mg (NO
3)
26H
2O, 73mLEu (NO
3)
3Solution (0.1M concentration), 9.9595 gram H
2C
2O
42H
2O, the spherical AACH powder of 20 grams, all the other are with embodiment 1.
Embodiment 8
Take by weighing 9.7490 gram Ba (NO
3)
2, 11.2815 gram Mg (NO
3)
26H
2O, 54.7mLEu (NO
3)
3Solution (0.1M concentration), 9.4062 gram H
2C
2O
42H
2O, the spherical AACH powder of 50 grams, all the other are with embodiment 1.
Claims (5)
1. the preparation method of an aluminate base blue colour fluorescent powder is characterized in that preparation process comprises:
A. with Ba (NO
3)
2And Mg (NO
3)
26H
2O is mixed with settled solution with deionized water, gets solution A; Wherein the concentration of barium and magnesium ion is 0.05～2mol/L;
B. with Eu (NO
3)
3Solution adds to solution A, stirs, and it is mixed, and gets solution B;
C. spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the deionized water, gets suspension C;
D. in suspension C, add H then
2C
2O
42H
2O stirs, and makes it to dissolve fully, gets suspension D;
E. the pH value with NaOH solution adjusting suspension D is 8.5～11, solution B is at the uniform velocity added among the suspension D, by the chemical constitution preparing metal ionic B of the aluminate base blue colour fluorescent powder that will prepare and the mixing solutions of D, barium and magnesium raw material are with respect to aluminium excessive 1%～100%, stirring reaction, regulating control pH with NaOH solution is 8.5～11; Behind the reinforced end of processing, behind the continuation stirring reaction, staticly settle, with the throw out deionized water wash, dehydration, oven dry obtains fluffy powder;
F. the powder roasting after will drying makes aluminate base blue colour fluorescent powder.
2. the preparation method of a kind of aluminate base blue colour fluorescent powder according to claim 1 is characterized in that spherical Aluminum Carbonate Basic ammonium AACH powder is scattered in the suspension that forms in the deionized water, and the system solid content is 20～100g/L; Add H
2C
2O
42H
2O and NaOH stir as precipitation agent, and system pH is controlled between 8.5～11.
3. the preparation method of a kind of aluminate base blue colour fluorescent powder according to claim 1, it is characterized in that the mixing solutions B of metal ion is at the uniform velocity joined among the AACH powder suspension D by peristaltic pump, feed rate is controlled at 5～20mL/min, stir simultaneously, solution B at the uniform velocity adds the pH value of the precipitation system behind the suspension D between 8.5～11.
4. the preparation method of a kind of aluminate base blue colour fluorescent powder according to claim 1, after the mixing solutions B that it is characterized in that metal ion dropwises, the precipitation system that solution B adds behind the suspension D continues to stir 1～5 hour, then stop to stir, leave standstill, suction filtration, washing, dehydration, oven dry, obtain fluffy powder.
5. the preparation method of a kind of aluminate base blue colour fluorescent powder according to claim 1, it is characterized in that dried powder roasting temperature of 1200 to 1500 ℃ in reducing atmosphere is promptly obtained required blue colour fluorescent powder after 1～6 hour, wherein reducing atmosphere is provided by the carbon dust burning, or uses nitrogen/hydrogen mixed gas.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101093687A CN100506946C (en) | 2006-08-14 | 2006-08-14 | Preparation method of aluminate base blue color fluorescent powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101093687A CN100506946C (en) | 2006-08-14 | 2006-08-14 | Preparation method of aluminate base blue color fluorescent powder |
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| Publication Number | Publication Date |
|---|---|
| CN1903978A CN1903978A (en) | 2007-01-31 |
| CN100506946C true CN100506946C (en) | 2009-07-01 |
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|---|---|---|---|
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1537918A (en) * | 2003-10-22 | 2004-10-20 | 袁曦明 | High-brightness small blue luminous particle and its preparation method |
| CN1664057A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Process for preparing aluminate fluorescent powder by coprecipitation method |
-
2006
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| CN1537918A (en) * | 2003-10-22 | 2004-10-20 | 袁曦明 | High-brightness small blue luminous particle and its preparation method |
| CN1664057A (en) * | 2005-02-21 | 2005-09-07 | 东南大学 | Process for preparing aluminate fluorescent powder by coprecipitation method |
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| 共沉淀法制备长余辉发光材料SrAl2O4:Eu2+,Dy3+的研究. 袁曦明等.材料开发与应用，第17卷第2期. 2002 |
| 共沉淀法制备长余辉发光材料SrAl2O4:Eu2+,Dy3+的研究. 袁曦明等.材料开发与应用，第17卷第2期. 2002 * |
| 长余辉发光材料研究进展. 欧得华等.江苏化工 33 4，第33卷第4期. 2005 |
| 长余辉发光材料研究进展. 欧得华等.江苏化工 33 4，第33卷第4期. 2005 * |
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