CN1295297C - Alumina coated fluorescent powder and its coating method - Google Patents
Alumina coated fluorescent powder and its coating method Download PDFInfo
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- CN1295297C CN1295297C CNB200510037843XA CN200510037843A CN1295297C CN 1295297 C CN1295297 C CN 1295297C CN B200510037843X A CNB200510037843X A CN B200510037843XA CN 200510037843 A CN200510037843 A CN 200510037843A CN 1295297 C CN1295297 C CN 1295297C
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Abstract
Aluminium oxide coating fluorescent powder is prepared by that an Al2O3 film is coated on the surface of fluorescent powder. A coating method comprises the following steps that a conjugate acid-alkali system whose pH value ranges from 4.5 to 6.0 is prepared into buffering liquid whose concentration is more than 0.1M and is less than 2M, the weight ratio of Al2O3 to fluorescent powder is from 0.25 to 20: 100, and a corresponding amount of water-soluble aluminium salt is weighed and is prepared into water-soluble aluminium salt solution with the concentration of 0.01 to 1.0M; then, fluorescent powder is added to the buffering liquid so as to prepare fluorescent powder suspending liquid with the concentration of 0.2 to 5%, and the fluorescent powder suspending liquid is stirred and dispersed by supersonic waves so that the fluorescent powder is completely dispersed in the buffering liquid; next, the fluorescent powder suspending liquid is heated to 20 to 60 DEG C and is stirred at the speed of 100 r/m to 300 r/m, and the water-soluble aluminium salt solution is dripped into the fluorescent powder suspending liquid at the dripping speed of 5 to 500 ml/min; then, temperature continues to be maintained, and a mixed solution of the water-soluble aluminium salt solution and the fluorescent powder suspending liquid continues to be stirred for 30 to 120 minutes; finally, a pH value of mother liquid is regulated to 6 to 7 by an alkaline solution so as to obtain coating alumina hydrate, the coating alumina hydrate is separated, washed, dehydrated and dried at 60 to 120 DEG C so that the water content of coating fluorescent powder is less than 0.25%, and the coating fluorescent powder is burned for 1 to 3 hours at 200 to 400 DEG C and is cooled in air together with a furnace so as to obtain the aluminium oxide coating fluorescent powder.
Description
Technical field
The present invention relates to a kind of fluorescent material, relate in particular to a kind of aluminum oxide coated fluorescent powder and film method for coating thereof that is used for plasma panel display spare.
Background technology
(Plasma Display Panel PDP) is vacuum ultraviolet ray (VUV) excitated fluorescent powder that utilizes inert mixed gas (claiming penning gas again) discharge generation to the chromatic plasma flat-panel monitor, realizes now looking like purpose.PDP is 100～200nm with the excitation wavelength range of fluorescent material, and main excitation band is near 147nm and 172nm.
The composition of the red-green-blue fluorescent material in the most frequently used PDP of being used for field is at present: rouge and powder (Y
2O
3: Eu
3+, (Y, Gd) BO
3: Eu
3+), green powder (ZnSiO
4: Mn
2+, BaAl
12O
19: Mn
2+), blue powder (BaMgAl
10O
17: Eu
2+) these several fluorescent material since its have good illumination efficiency and chemical stability, be widely used in the plasma display field.
But owing in order to satisfy the requirement that PDP is coated with screen, need PDP to have less granularity (2～4 μ m) with fluorescent material, the granularity of the more general used fluorescent material of lighting source (6～8 μ m) is much smaller.The most frequently used preparation technology remains and adopts high temperature solid-state method to carry out the synthetic of fluorescent material at present, initial particle size after synthetic generally all will be more than 6～7 microns, in order to satisfy granularity requirements, must carry out dispersion and fining to fluorescent material, thereby damaged phosphor surface, caused surface crystallinity obviously to descend.And the fluorescent powder grain that this surface has a damage is very easily oxidized in follow-up system screen thermal treatment, causes luminescent properties to descend.On the other hand, because the photon energy of the excitation wavelength of fluorescent material 147nm is much higher than 254nm shortwave ultraviolet in the traditional lighting light source and the sub-energy of 365nm long wave ultraviolet light in the PDP indicating meter, under the vacuum ultraviolet excitation of this high energy, PDP can also can produce significant light decay with fluorescent material, and energetic ion has also caused the work deterioration of fluorescent material to the bombardment of phosphor surface simultaneously.The effect of this two aspects factor all causes the shortening greatly in the work-ing life of fluorescent material and PDP device, has influenced the performance of PDP display performance.
And to improve the thermostability and the anti-work deteriorate performance thereof of fluorescent material, fluorescent material is carried out the surface coat that to handle be a kind of efficient ways.Adopt general fluorescent material coating technology, to the protection poor effect of thermal degradation when especially VUV radiation deterioration.The sol-gel method more as present research, although this method technology is simple, easy to operate, but coating layer is inhomogeneous, be difficult to the controlling packet coating thickness, and in heat-processed, very easily reunite this peplos excessive cycle between the powder, operation is many, is difficult to realize that industrialization also is the weak point of its existence.
Summary of the invention
The invention provides a kind of heat resistanceheat resistant deterioration that can improve chromatic plasma flat-panel monitor fluorescent material and anti-work deteriorate performance and help the aluminum oxide coated fluorescent powder and the film method for coating thereof of industrialization, the coating of phosphor surface of the present invention has the advantage of continuous even compact.
The present invention adopts following technical scheme:
The technical scheme of described aluminum oxide coated fluorescent powder is as follows:
The aluminum oxide coated fluorescent powder that a kind of chromatic plasma flat-panel monitor is used is characterized in that being coated with Al at phosphor surface
2O
3Film.
The technical scheme of described film method for coating is as follows:
A kind of film method for coating that is used to implement above-mentioned aluminum oxide coated fluorescent powder:
1) adopt the pH value be in concentration that conjugate acid and base system between 4.5～6.0 is made into damping fluid and this damping fluid greater than 0.1M less than 2M, press Al
2O
3With the weight ratio of fluorescent material be (0.25～20): 100 ratios take by weighing the water-soluble aluminum salt of respective amount and are mixed with the water-soluble aluminum salts solution that concentration is 0.01～1.0M;
2) the chromatic plasma flat-panel monitor is put into damping fluid with fluorescent material, be made into concentration and be 0.2～5% phosphor suspension, stir ultra-sonic dispersion 10～30min simultaneously, fluorescent material is well dispersed in the damping fluid;
3) phosphor suspension is heated to 20～60 ℃, speed with 100r/m～300r/min stirs, slowly splash into the water-soluble aluminum salts solution in the phosphor suspension simultaneously, rate of addition is 5～500ml/min, finish follow-up continuation of insurance mild stirring 30～120min, regulate mother liquor pH value to 6～7 with alkaline solution at last, form the hydrated alumina coating on the fluorescent material in phosphor suspension;
4) with the capsule luminescent powder suspension centrifugation, washing, dehydration; Then, 60～120 ℃ of oven dry down, the water ratio that makes coated fluorescent powder is less than 0.25%; Carry out 200～400 ℃ of calcination 1～3h at last,, obtain the aluminum oxide coated fluorescent powder with the stove air cooling.
Compared with prior art, the present invention has following advantage:
(1) the coating reaction process is easy to control; Utilize the characteristic of damping fluid Al (OH) can be controlled in the pH of suspension value stabilization ground of fluorescent material
3Take place in the required pH value scope of heterogeneous forming core, simultaneously by control Al (NO
3)
3The rate of addition of solution is effectively controlled Al (OH)
3The nucleation rate and the speed of growth.
(2) because in certain scope, membrane wrapping thickness increases with the increase of coating material consumption, therefore by regulating the part by weight of coating material and fluorescent material, the effectively thickness of controlling packet rete;
(3) because the coating reaction is what to carry out with the mechanism of heterogeneous forming core, it is hereby ensured that the coating material is at first at the phosphor surface forming core, and the ion that guarantees the coating material by quick stirring is dispersed in the whole suspension system, thereby can guarantee rete evenly growth continuously;
(4) because the coating material is coated on phosphor surface in the mode of chemical bonding, so membranous layer binding force is strong, difficult drop-off;
(5) because coating layer is even continuously, therefore can effectively be isolated in the intrusion of extraneous oxygen [O] in the fluorescent material calcination process, thereby have avoided excitation center Eu in the fluorescent material
2+Be oxidized to Eu
3+In the PDP working order, coating is isolated the bombardment of energetic ion and the direct irradiation of ultraviolet ray (UV) or vacuum ultraviolet ray (VUV), thereby has significantly improved the heat resistanceheat resistant deterioration and the anti-work deteriorate performance of fluorescent material.
(6) adopt Al
2O
3Form composite coatedly with other oxide compounds, can have the better protection effect.
(7) present method shortened greatly than the sol-gel method craft cycle, and cost significantly reduces, and was easier to realize industrialization.
Description of drawings
Fig. 1 is surrounded by Al
2O
3Coating and coating Al not
2O
3Coating BaMgAl
12O
19: Eu
2+(BAM) the blue powder relative brightness (a) is coating BAM blue powder with the variation relation figure of calcination temperature; (b) be coating BAM blue powder not.
Embodiment
Embodiment 1
The aluminum oxide coated fluorescent powder that a kind of chromatic plasma flat-panel monitor is used is characterized in that being coated with Al at phosphor surface
2O
3Film is at Al
2O
3Film is outer can select to coat TiO again
2Film, In
2O
3Film, ZrO
2Film or rare earth oxide La
2O
3Film also can coat successively entirely, in the present embodiment, and at Al
2O
3Be coated with TiO on the film
2Film coats In again at phosphor surface
2O
3Film coats ZrO again at phosphor surface
2Film, last, coat La at phosphor surface
2O
3
Embodiment 2
A kind of film method for coating that is used to implement above-mentioned aluminum oxide coated fluorescent powder:
1) adopt the pH value be in concentration that conjugate acid and base system between 4.5～6.0 is made into damping fluid and this damping fluid greater than 0.1M less than 1M, press Al
2O
3With the weight ratio of fluorescent material be (0.25～20): 100 ratios, in the present embodiment, can be by Al
2O
3With the weight ratio of fluorescent material be 0.25: 100,15: 100,2: 100,7: 100, or 12: 100 ratio, take by weighing the water-soluble aluminum salt of respective amount and be mixed with the water-soluble aluminum salts solution that concentration is 0.01～1.0M, for example: being mixed with concentration is 0.01M, 1M, 0.07M, 0.12M, 0.56M or the water-soluble aluminum salt volumetric soiutions of 0.82M, above-mentioned conjugate acid and base system can be the pH value be 4.75 and concentration be acetate-sodium acetate conjugate acid and base system of 0.1M, the pH value be 5.0 and concentration be the citric acid-NaOH conjugate acid and base system of 1.0M or pH value be 5.5 and concentration be Potassium Hydrogen Phthalate-NaOH conjugate acid and base system of 0.58M, water-soluble aluminum salt can be Al (NO
3)
39H
2O, AlCl
36H
2O or Al
2(SO
4)
318H
2O;
2) the chromatic plasma flat-panel monitor is put into damping fluid with fluorescent material, be made into concentration and be 0.2～5% phosphor suspension, as: be mixed with concentration and be 0.2,0.29,0.85,1.5 or 2% phosphor suspension, stir ultra-sonic dispersion 10～30min simultaneously, as: ultra-sonic dispersion 10min, 30min, 18min or 25min are well dispersed in the damping fluid fluorescent material;
3) phosphor suspension is heated to 20～60 ℃, speed with 100r/m～300r/m stirs, this temperature may be selected to be 20 ℃, 70 ℃, 33 ℃, 47 ℃ or 62 ℃, this speed may be selected to be 100r/m, 300r/m, 170r/m, 230r/m, 240r/m or 280r/m, slowly splash into the water-soluble aluminum salts solution in the phosphor suspension simultaneously, rate of addition is 5～500ml/min, present embodiment can be selected 15ml/min, 11ml/min, 7ml/min, 4ml/min, 170ml/min, 277ml/min, 357ml/min, 458ml/min, the rate of addition of 500ml/min or 2ml/min, need to prove, when the fluorescent material amount that once coats more after a little while, as when having only 100g, can adopt single mouth or two mouth low speed to splash into, drip speed control and get final product with interior built in 5～15ml/min; And when the fluorescent material amount that once needs to coat is very big, as reached 1kg when above, in order to guarantee coating efficient, avoid simultaneously local potential of hydrogen too high and influence the coating quality again, should take the different zones simultaneously titration of many drip nozzles (as: more than 3) at reactor, to guarantee the homogeneity of whole system potential of hydrogen, and each drip nozzle still must drip with lower speed, rate of addition is controlled in 5～30ml/min, finish follow-up continuation of insurance mild stirring 30～120min, as: insulation and the time of stirring are 30,56,88,126,171 or 180min, regulate mother liquor pH value to 6～7 with alkaline solution at last, form the hydrated alumina coating on the fluorescent material in phosphor suspension;
4) with the capsule luminescent powder suspension centrifugation, wash 2～4 times, dewater 1～3 time; Then, 60～120 ℃ of oven dry down, the water ratio that makes coated fluorescent powder is less than 0.25%; Carry out 200～400 ℃ of calcination 1～3h at last, with the stove air cooling, obtain the aluminum oxide coated fluorescent powder, above-mentioned bake out temperature can be selected 60,72,88,109 or 120 ℃, water ratio can select 0.25%, 0.20%, 0.15%, 0.04%, calcination can be selected 200 ℃ of calcination 3h, 300 ℃ of calcination 3h, 400 ℃ of calcination 1h.
In the present embodiment, before the chromatic plasma flat-panel monitor is carried out coating with fluorescent material, the chromatic plasma flat-panel monitor is dispersed in the alkali lye with fluorescent material, centrifugation behind immersion 6～72h, again it is washed to supernatant liquor and is neutral, specifically, can be dispersed in the chromatic plasma flat-panel monitor in the basic solution liquid such as sodium hydroxide, ammoniacal liquor with fluorescent material, centrifugation behind immersion 6～72h, for example: carry out 6,72,36,9,56 or 66h soak the back centrifugation, with distilled water or deionized water it is washed to supernatant liquor again and is neutral; Al
2O
3Consumption accounts for 1.0～5.0wt% of fluorescent material total amount; Present embodiment is by damping fluid phosphor suspension pH to be controlled in 4.75～5.25 scopes; The temperature of phosphor suspension is controlled at 30～40 ℃ in the coating process; The water-soluble aluminum salts solution finishes follow-up continuation of insurance mild stirring, and promptly digestion time is controlled at 30～60min scope with interior preferable; Coated fluorescent powder is put into baking oven or spray drying device, and drying temperature is controlled under 70～80 ℃, and with the fluorescent material oven dry, the water ratio that makes fluorescent material is less than 0.25%.
Embodiment 3
Take by weighing 50gPDP BaMgAl
10O
17: Eu
2+Fluorescent material (BAM) is put into the NaOH solution that concentration is 0.5M, soaks 24h, uses the separating centrifuge separating and dehydrating then, with the distilled water washing, is neutral until supernatant liquor again.
Take by weighing the 23gNaAc solid and be melted in a small amount of distilled water, add the dense HAc of 27ml then, add 0.1% tween 80 dispersion agent 5ml again, last thin up obtains the damping fluid of pH=4.5 to 500ml.Get 10g and be added in the damping fluid, use ultrasonic dispersing 10min, heating in water bath to 30 ℃ through the pretreated BAM blue powder of alkalescence.Take by weighing 1.88gAl (NO
3)
39H
2The O solid solution is made into 100ml solution, the speed of dripping with 5ml/min adds in the fluorescent material coating mother liquor, finish back ageing 30min, with concentration is the NaOH solution adjusting mother liquor pH value to 6.5 of 0.05M, and centrifugation is afterwards washed 2 times, dehydrated alcohol dehydration 2 times, 80 ℃ of oven dry are after 300 ℃ of calcinations obtain coating PDP BAM blue powder.
Embodiment 4
Take by weighing the 36gNaAc solid and be melted in a small amount of distilled water, add the dense HAc of 14ml then, add 0.025% tween 80 dispersion agent 5ml again, last thin up obtains the damping fluid of pH=5 to 500ml.Take by weighing 10g and be added in the damping fluid, ultrasonic dispersing 10min, heating in water bath to 30 ℃ through the pretreated BAM blue powder of alkalescence.Take by weighing 3.68gAl (NO
3)
39H
2The O solid solution is made into 150ml solution, the speed of dripping with 10ml/min adds in the fluorescent material coating mother liquor, finish back ageing 30min, with concentration is the NaOH solution adjusting mother liquor pH value to 7 of 0.05M, and centrifugation is washed 3 times, dehydrated alcohol dehydration 2 times, 100 ℃ of oven dry are after 250 ℃ of calcinations obtain coating PDP BAM blue powder.
Embodiment 5
High and the oxide compound Al that have fine consistency with aluminate fluorescent powder matrix to visible light and vacuum ultraviolet ray light permeable rate
2O
3With heterogeneous nucleation process, phosphor surface obtained one deck continuously, the coating of even compact, improved the performance of PDP fluorescent material heat resistanceheat resistant deterioration and anti-work deterioration.PDP fluorescent material cladding process step of the present invention is as follows:
1, PDP fluorescent material pre-treatment
PDP fluorescent material is dispersed in the NaOH solution that concentration is 0.1M～1.0M soaks 6～72h, use the separating centrifuge separating and dehydrating then, use distilled water (or deionized water) washing again, be neutral until supernatant liquor.
2, preparation pH damping fluid and coating substance solution
(or citric acid-NaOH, the conjugate acid and base system of Potassium Hydrogen Phthalate-NaOH) take by weighing the acetate and the sodium acetate of corresponding weight, are mixed with the damping fluid between pH=4.5～6 to adopt acetate-sodium acetate (HAc-NaAc).Press Al
2O
3/ fluorescent material weight ratio=0.25～10% takes by weighing the Al (NO of respective amount
3)
39H
2O (or AlCl
36H
2O, Al
2(SO
4)
318H
2O) be mixed with the solution that concentration is 0.01～0.5M.
3, preparation phosphor suspension
To put into pH value damping fluid through the pretreated PDP fluorescent material of alkalescence, compound concentration is 0.2～5% phosphor suspension, stirs 10～30min in the time of ultra-sonic dispersion, guarantees that fluorescent material is well dispersed in the damping fluid.
4, coating
With 20～60 ℃ of coating mother liquor heating in water bath, the while vigorous stirring, stirring velocity is controlled between 100r/m～200r/m.With Al (NO
3)
3Solution slowly splashes in the mother liquor, and finishing back ageing 30～120min is NaOH (or the NH of 0.05～1.0M at last with concentration
3H
2O) aqueous solution is regulated mother liquor pH value to 6～7.
5, aftertreatment
With the coated fluorescent powder centrifugation after the ageing, use distilled water (or deionized water) washing 2～4 times again, dehydrated alcohol dehydration 1～3 time.Put into 60～120 ℃ of oven dry of baking oven then, preferable with 70～80 ℃.Control coated fluorescent powder water ratio is less than 0.5%.Carry out 200～400 ℃ of low temperature calcinations at last, with the stove air cooling.
Claims (5)
1, a kind of film method for coating that is used for the aluminum oxide coated fluorescent powder that the chromatic plasma flat-panel monitor uses is characterized in that:
1) adopt the pH value be in concentration that conjugate acid and base system between 4.5～6.0 is made into damping fluid and this damping fluid greater than 0.1M less than 2M, press Al
2O
3With the weight ratio of fluorescent material be (0.25～20): 100 ratios take by weighing the water-soluble aluminum salt of respective amount and are mixed with the water-soluble aluminum salts solution that concentration is 0.01～1.0M;
2) the chromatic plasma flat-panel monitor is put into damping fluid with fluorescent material, be made into concentration and be 0.2～5% phosphor suspension, stir ultra-sonic dispersion 10～30min simultaneously, fluorescent material is well dispersed in the damping fluid;
3) phosphor suspension is heated to 20～60 ℃, speed with 100r/m～300r/m stirs, slowly splash into the water-soluble aluminum salts solution in the phosphor suspension simultaneously, rate of addition is 5～500ml/min, finish follow-up continuation of insurance mild stirring 30～120min, regulate mother liquor pH value to 6～7 with alkaline solution at last, form the hydrated alumina coating on the fluorescent material in phosphor suspension;
4) with the capsule luminescent powder suspension centrifugation, washing, dehydration; Then, 60～120 ℃ of oven dry down, the water ratio that makes coated fluorescent powder is less than 0.25%; Carry out 200～400 ℃ of calcination 1～3h at last,, obtain the aluminum oxide coated fluorescent powder with the stove air cooling.
2, by the described film method for coating of claim 1, it is characterized in that before the chromatic plasma flat-panel monitor is put into damping fluid with fluorescent material, the chromatic plasma flat-panel monitor is dispersed in the alkali lye with fluorescent material, centrifugation behind immersion 6～72h, again it is washed to supernatant liquor and is neutral, Al
2O
3Consumption accounts for 1.0～5.0wt% of fluorescent material total amount.
3, by the described film method for coating of claim 1, it is characterized in that phosphor suspension pH being controlled in 4.75～5.25 scopes by damping fluid.
4, by the described film method for coating of claim 1, it is characterized in that the temperature of phosphor suspension in the coating process is controlled at 30～40 ℃.
5, by the described film method for coating of claim 1, it is characterized in that coated fluorescent powder puts into baking oven or spray drying device, drying temperature is controlled under 70～80 ℃, and with the fluorescent material oven dry, the water ratio that makes fluorescent material is less than 0.25%.
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|---|---|---|---|
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|---|---|---|---|
| CNB200510037843XA CN1295297C (en) | 2005-02-25 | 2005-02-25 | Alumina coated fluorescent powder and its coating method |
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| CN1295297C true CN1295297C (en) | 2007-01-17 |
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| CN100363457C (en) * | 2005-11-04 | 2008-01-23 | 中国科学院长春应用化学研究所 | Low heat solid phase method for implementing nano-cladding on fluorescent pewder surface |
| CN102719235A (en) * | 2012-03-12 | 2012-10-10 | 苏州英特华照明有限公司 | La2O3 coated LED phosphor particle and preparation method thereof |
| CN102690647A (en) * | 2012-05-23 | 2012-09-26 | 苏州英特华照明有限公司 | Cold cathode green phosphor for composite oxide coating and preparation method therefor |
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| CN103275708B (en) * | 2013-02-28 | 2016-06-15 | 福建省长汀金龙稀土有限公司 | A kind of surface-coating method of lamp BAM fluorescent material |
| CN104556161A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Flaky gamma-Al2O3 nanometer crystal and preparation method thereof |
| CN104130770A (en) * | 2014-06-30 | 2014-11-05 | 彩虹集团电子股份有限公司 | Surface treatment method of high luminous efficiency white light LED (light-emitting diode) use orange fluorescent powder |
| CN109133878B (en) * | 2017-06-28 | 2021-11-30 | 深圳光峰科技股份有限公司 | Composite ceramic and preparation method thereof |
| CN110386820B (en) * | 2018-04-19 | 2021-02-26 | 深圳光峰科技股份有限公司 | Aluminum oxynitride matrix fluorescent ceramic and preparation method thereof |
| CN111334281B (en) * | 2020-03-06 | 2023-07-04 | 英特美光电（苏州）有限公司 | Preparation method of composite coated yellow fluorescent powder special for COB |
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| CN1261394A (en) * | 1997-06-30 | 2000-07-26 | 美国3M公司 | Electroluminescent phosphor particles encapsulated with an aluminum oxide based multiple oxide coating |
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| CN1468936A (en) * | 2003-06-10 | 2004-01-21 | 山东宇光电子科技有限公司 | Electroluminescent composite coated ZnS:Cu/Cu.Mn material and its prepn process |
| CN1498257A (en) * | 2001-09-12 | 2004-05-19 | ���µ�����ҵ��ʽ���� | Phosphor manufacturing method thereof and plasma display apparatus |
-
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- 2005-02-25 CN CNB200510037843XA patent/CN1295297C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1261394A (en) * | 1997-06-30 | 2000-07-26 | 美国3M公司 | Electroluminescent phosphor particles encapsulated with an aluminum oxide based multiple oxide coating |
| CN1275153A (en) * | 1998-08-25 | 2000-11-29 | 皇家菲利浦电子有限公司 | Method of coating luminescent material |
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