CN1664052A - Silicon oxide coated fluorescent powder and its coating method - Google Patents
Silicon oxide coated fluorescent powder and its coating method Download PDFInfo
- Publication number
- CN1664052A CN1664052A CN 200510037844 CN200510037844A CN1664052A CN 1664052 A CN1664052 A CN 1664052A CN 200510037844 CN200510037844 CN 200510037844 CN 200510037844 A CN200510037844 A CN 200510037844A CN 1664052 A CN1664052 A CN 1664052A
- Authority
- CN
- China
- Prior art keywords
- coating
- phosphor powder
- suspension
- phosphor suspension
- fluorescent material
- 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.)
- Granted
Links
Images
Landscapes
- Luminescent Compositions (AREA)
Abstract
Disclosed is the silicon oxide integument phosphor powder covered with silicon oxide on the surface of the phosphor powder. The method of integument comprising: preparing suspension at the concentration 0.2~5% with color plasma panel display phosphor powder and water, weighing relevant quantity of sodium silicate with nine water according to the proportion between silicon oxide and phosphor powder by weight (0.5~20): 100, adding to the phosphor powder suspension, dispersing with supersonic wave and stirring to make it dissolved and the phosphor powder suspension stable, employing strong acid as precipitator and preparing solution with concentration 0.01~2M; heating the phosphor powder suspension to 20~120 DEG C, stirring and dispersing with supersonic wave at the same time, stirring with speed 100r/m~ 300r/m and dropping the precipitator into the phosphor powder suspension at the speed of 5~500ml/min to make the pH value 3~11, then keeping the temperature and stirring for 30~180 minutes; getting the integument phosphor powder after centrifugalizating the phosphor powder suspension, washing, dewatering and drying at 60-120DEG C to make the integument phosphor powder moisture percentage below 0.25%,incandescing at 200~400 DEG C for 1~3hours and air cooling in the furnace.
Description
Technical field
The present invention relates to a kind of chromatic plasma flat-panel monitor with fluorescent material and relevant treatment process, relate in particular to a kind of chromatic plasma flat-panel monitor silicon oxide coated fluorescent powder and coating method thereof.
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 100～200mm with the excitation wavelength range of fluorescent material, and main excitation band is near 147nm and 172nm.
The composition of the three primary colors fluorescent powder in the most frequently used PDP of being used for field has 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 aluminate blue powder (BaMgAl wherein
10O
17: Eu
2+) and green powder (BaAl
12O
19: Mn
2+) exist comparatively significantly deterioration problem.This comprises operation deterioration and work deterioration two aspects.On the one hand, mainly be because the bisque of PDP about needing through 500 ℃ in system screen process solidifies sintering circuit, caused the luminescent properties deterioration of aluminate blue powder and green powder, be embodied in luminosity and significantly descend, chromaticity coordinates drifts about.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.Patent CN1506438A is actual to be to adopt colloidal sol that PDP fluorescent material is coated, although this method technology is simple, easy to operate, coating layer is inhomogeneous, is difficult to the controlling packet coating thickness.Even situation about coating not on takes place, the mechanically mixing of just be covered powder and coating material micelle.
Summary of the invention
The chromatic plasma flat-panel monitor that the invention provides a kind of heat resistanceheat resistant deterioration that can effectively improve PDP fluorescent material and anti-work deteriorate performance, the continuous even compact of phosphor surface coating is with silicon oxide coated fluorescent powder and coating method thereof, and the present invention can effectively improve the luminescent properties of fluorescent material.
The present invention adopts following technical scheme:
The chromatic plasma flat-panel monitor that the present invention relates to is as follows with the coated fluorescent powder technical scheme:
A kind of chromatic plasma flat-panel monitor coated fluorescent powder contains SiO in the phosphor surface coating
2Coating.
The chromatic plasma flat-panel monitor that the present invention relates to is as follows with the coating method technical scheme of coated fluorescent powder:
1) chromatic plasma flat-panel monitor fluorescent material being made into concentration with distilled water is 0.2～2% phosphor suspension, presses SiO
2With fluorescent material be (0.5～20): 100 mass ratio takes by weighing the Na of respective amount
2SiO
39H
2O, and add phosphor suspension, ultra-sonic dispersion also stirs 10～30min, makes Na
2SiO
3Dissolving also makes phosphor suspension be in steady state, with HCl, HNO
3Or H
2SO
4Be precipitation agent, being made into concentration is 0.01～2M solution;
2) phosphor suspension is heated to 20～120 ℃, stir ultra-sonic dispersion 10～30min simultaneously, stirring velocity is 100～300r/m, rate of addition with 5～500ml/min splashes into phosphor suspension with precipitation agent, make its pH value to 3～10, titration finishes the back phosphor suspension is continued insulation and stirs 30～180min;
3) will obtain coated fluorescent powder after the capsule luminescent powder suspension centrifugation,, under 60～120 ℃, coated fluorescent powder is dried to its water ratio less than 0.25% then its washing, dehydration; At last at 200～400 ℃ of following calcination 1～3h, with the stove air cooling.
Compared with prior art, the present invention has following advantage:
(1) the coating reaction process is easy to control, by regulating the concentration and the rate of addition of precipitation agent, can effectively control Na
2SiO
3Hydrolysis rate, and then form, the thickness of coating layer controlled;
(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) owing in the coating reaction process, coating material SiO
2Hydrate polyreaction has taken place at phosphor surface, so rete is fine and close continuously, and coating is combined in phosphor surface in the mode of chemical bonding, so membranous layer binding force is strong, difficult drop-off; SiO
2The oxide compound coating has good weatherability properties and to visible light and vacuum ultraviolet ray light permeable rate height.
(5), therefore can effectively be isolated in the intrusion of extraneous oxygen [O] in the fluorescent material calcination process, thereby avoid excitation center Eu in the fluorescent material owing to the continuous even compact of coating layer
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 SiO
2With ZrO
2Or the composite coated weathering resistance and the protection effect that can further improve fluorescent material of other oxide compounds formations.
(7) present method is compared with additive methods such as sol-gel methodes with alkoxide hydrolysis, and process cycle shortens greatly, and cost significantly reduces, and is easier to realize industrialization.
Description of drawings
Fig. 1 is a coating and coating BaMgAl not
12O
19: the relative brightness of Eu2+ blue powder is with the variation relation of calcination temperature, (a) the BAM blue powder of coating; (b) the BAM blue powder of coating not.
Fig. 2 is the transmission electron microscope of coated fluorescent powder of the present invention.
Embodiment
Embodiment 1
A kind of chromatic plasma flat-panel monitor silicon oxide coated fluorescent powder contains SiO in the phosphor surface coating
2Coating, at SiO
2The coating outside can also coat La again
2O
3And ZrO
2, constitute composite coated, in the present embodiment, at SiO
2The outside of coating coats ZrO
2Coating coats La again in the outside of fluorescent material coating
2O
3Coating.
Embodiment 2
A kind of coating method that is used to prepare above-mentioned coated fluorescent powder:
1) chromatic plasma flat-panel monitor fluorescent material being made into concentration with distilled water is 0.2～5% phosphor suspension, presses SiO
2With fluorescent material be (0.5～20): 100 mass ratio takes by weighing the Na of respective amount
2SiO
39H
2O, and add phosphor suspension, ultra-sonic dispersion also stirs 10～30min, makes Na
2SiO
3Dissolving also makes phosphor suspension be in steady state, with HCl, HNO
3Or H
2SO
4Be precipitation agent, being made into concentration is 0.01～2M solution, above-mentioned SiO
2Can select 05: 100,20: 100,1.5: 100,5: 100,6.4: 100,8: 100,10: 100,13: 100 or 16: 100 with the mass ratio of fluorescent material, and SiO
2Consumption be good with the 5～10wt% that accounts for the fluorescent material total mass, the concentration of above-mentioned precipitation agent can select 0.05,0.1,0.5 or 1M; Before the preparation phosphor suspension, chromatic plasma flat-panel monitor fluorescent material is dispersed in the alkali lye, soaks centrifugation after 6～72 hours, again it is washed to supernatant liquor and is neutral, specifically, chromatic plasma flat-panel monitor fluorescent material is dispersed in the NaOH solution, soaks centrifugation after 6～72 hours, again it is washed to supernatant liquor and is neutral, in the present embodiment, the pH value can select 8,9,10, or 14, soak time can be selected 6,12,24 or 72 hours;
2) phosphor suspension is heated to 20～120 ℃, stir ultra-sonic dispersion 10～30min simultaneously, stirring velocity is 100～300r/m, rate of addition with 5～500ml/min splashes into phosphor suspension with precipitation agent simultaneously, regulate pH value to 3～11 of phosphor suspension and can select 3.5,6.2,7.5,8.6 or 10.4, titration finishes the back phosphor suspension continuation insulation and stirring is ageing 30～180min and can selects 30,180,46,79,96,147 or 169min, above-mentioned phosphor suspension Heating temperature can select 20,120,43,68,89 or 110 ℃, ultra-sonic dispersion 10,30,15,20 or 26min, stirring velocity is 100,125,175,200,250 or 300r/m, the rate of addition of precipitation agent can select 2,20,6,12,16,58,96,178,265,320,410 or 500ml/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, the speed control that drips of each drip nozzle gets 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, guaranteeing the homogeneity of whole system potential of hydrogen, and each drip nozzle still must drip with lower speed, and rate of addition is controlled in 5～30ml/min;
3) will obtain coated fluorescent powder after the capsule luminescent powder suspension centrifugation,, under 60～120 ℃, coated fluorescent powder is dried to its water ratio less than 0.25% then its washing, dehydration; At last at 200～400 ℃ of following calcination 1～3h, with the stove air cooling.
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 through the pretreated PDP fluorescent material of alkalescence BaMgAl
10O
17: Eu
2+Blue powder 10g puts into a small amount of distilled water, ultra-sonic dispersion 30min.Press SiO
2/ fluorescent material=2.5wt% ratio takes by weighing 1.18gNa
2SiO
39H
2O adds phosphor suspension, and adds 0.1% tween 80 dispersion agent 5ml in phosphor suspension, and last thin up stirs 30min and obtains homodisperse coating mother liquor to 500ml.With mother liquor heating in water bath to 60 ℃ and insulation, (stirring velocity: 200r/m), be that the HCl solution of 0.25M slowly splashes into mother liquor and equals 6～9 to the pH value with concentration, rate of addition is 10ml/min to carrying out vigorous stirring to mother liquor.Finish back ageing 120min, continue simultaneously to stir.After the end, centrifugation, distilled water (or deionized water) washing 2 times, dehydrated alcohol dehydration 2 times, again through 100 ℃ of oven dry, after 250 ℃ of calcinations obtain coating chromatic plasma flat-panel monitor (PDP) and use BAM blue powder.
Embodiment 4
Take by weighing through the pretreated PDP fluorescent material of alkalescence BaMgAl
10O
17: Eu
2+Blue powder 10g puts into a small amount of distilled water, ultra-sonic dispersion 30min.Press SiO
2/ fluorescent material=7.5wt% ratio takes by weighing 3.55gNa
2SiO
39H
2O adds phosphor suspension, and adds 0.1% tween 80 dispersion agent 5ml in phosphor suspension, and last thin up stirs 30min and obtains homodisperse coating mother liquor to 500ml in the time of ultra-sonic dispersion.Stir 0.5h and fully dissolve, and in phosphor suspension, add 0.2% tween 80 dispersion agent 2ml, obtain homodisperse mother liquor.With mother liquor heating in water bath to 80 ℃ and insulation, (stirring velocity: in the time of 20r/m) be that the HCl solution of 0.1M slowly splashes into mother liquor to pH value and equals 6～9 with concentration, rate of addition is 8ml/min to carrying out vigorous stirring to mother liquor.Finish back ageing 90min, continue simultaneously to stir.Subsequent step is the same.
Claims (8)
1, a kind of chromatic plasma flat-panel monitor silicon oxide coated fluorescent powder is characterized in that at phosphor surface coated Si O
2Coating.
2, silicon oxide coated fluorescent powder according to claim 1 is characterized in that at SiO
2The outside of coating coats ZrO
2Coating.
3, silicon oxide coated fluorescent powder according to claim 1 and 2 is characterized in that coating La again in the outside of fluorescent material coating
2O
3Coating.
4, a kind of coating method that is used to prepare the described coated fluorescent powder of claim 1 is characterized in that:
1) chromatic plasma flat-panel monitor fluorescent material being made into concentration with distilled water is 0.2～5% phosphor suspension, presses SiO
2With fluorescent material be (0.5～20): 100 weight ratio takes by weighing the Na of respective amount
2SiO
39H
2O, and add phosphor suspension, ultra-sonic dispersion also stirs 10～30min, makes Na
2SiO
3Dissolving also makes phosphor suspension be in steady state, with HCl, HNO
3Or H
2SO
4Be precipitation agent, be made into the solution that concentration is 0.01～2M;
2) phosphor suspension is heated to 20～120 ℃, stir ultra-sonic dispersion 10～30min simultaneously, rotating speed with 100～300r/m stirs phosphor suspension, rate of addition with 5～500ml/min splashes into phosphor suspension with precipitation agent simultaneously, make its pH value to 3～11, titration finishes the back phosphor suspension is continued insulation and stirs 30～180min;
3) will obtain coated fluorescent powder after the capsule luminescent powder suspension centrifugation,, under 60～120 ℃, coated fluorescent powder is dried to its water ratio less than 0.25% then its washing, dehydration; At last at 200～400 ℃ of following calcination 1～3h, with the stove air cooling.
5, by the described coating method of claim 4, it is characterized in that before the preparation phosphor suspension, chromatic plasma flat-panel monitor fluorescent material being dispersed in the alkali lye, soak centrifugation after 6～72 hours, again it is washed to supernatant liquor and is neutral, SiO
2Consumption account for 5～10wt% of fluorescent material total mass.
6, by claim 4 or 5 described chromatic plasma flat-panel monitors fluorescent material coating treatment process, it is characterized in that precipitation agent is splashed into phosphor suspension, make its pH value to 6～9.
7,, carry out precipitation agent after it is characterized in that phosphor suspension is heated to 40～80 ℃ and drip by the described coating method of claim 6.
8,, it is characterized in that precipitation agent drips the end back phosphor suspension is continued insulation and stirs 60～120min by the described coating method of claim 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037844 CN1286941C (en) | 2005-02-25 | 2005-02-25 | Silicon oxide coated fluorescent powder and its coating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037844 CN1286941C (en) | 2005-02-25 | 2005-02-25 | Silicon oxide coated fluorescent powder and its coating method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1664052A true CN1664052A (en) | 2005-09-07 |
| CN1286941C CN1286941C (en) | 2006-11-29 |
Family
ID=35035369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510037844 Expired - Fee Related CN1286941C (en) | 2005-02-25 | 2005-02-25 | Silicon oxide coated fluorescent powder and its coating method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1286941C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665690B (en) * | 2009-09-23 | 2012-07-25 | 东南大学 | Preparation method of waterproof fluorescent powder |
| CN102660281A (en) * | 2012-05-28 | 2012-09-12 | 北京晶创达科技有限公司 | Silica-coated orange-red phosphor and preparation method thereof |
| 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 |
| 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 |
| CN105154061A (en) * | 2015-10-01 | 2015-12-16 | 上海洞舟实业有限公司 | Transparent damp-proof film wrapping method for electroluminescence powder |
| CN105462578A (en) * | 2015-11-27 | 2016-04-06 | 西南科技大学 | Novel SiO2/CaCO3-matrix red fluorescent powder and preparation method thereof |
-
2005
- 2005-02-25 CN CN 200510037844 patent/CN1286941C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665690B (en) * | 2009-09-23 | 2012-07-25 | 东南大学 | Preparation method of waterproof fluorescent powder |
| 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 |
| CN102660281A (en) * | 2012-05-28 | 2012-09-12 | 北京晶创达科技有限公司 | Silica-coated orange-red phosphor and preparation method thereof |
| 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 |
| CN105154061A (en) * | 2015-10-01 | 2015-12-16 | 上海洞舟实业有限公司 | Transparent damp-proof film wrapping method for electroluminescence powder |
| CN105462578A (en) * | 2015-11-27 | 2016-04-06 | 西南科技大学 | Novel SiO2/CaCO3-matrix red fluorescent powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1286941C (en) | 2006-11-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1295297C (en) | Alumina coated fluorescent powder and its coating method | |
| CN1286941C (en) | Silicon oxide coated fluorescent powder and its coating method | |
| Im et al. | A novel blue-emitting silica-coated KBaPO4: Eu2+ phosphor under vacuum ultraviolet and ultraviolet excitation | |
| CN105038776A (en) | Preparation method of Mn<4+> doped fluoride fluorescent powder material and method for surface modification of Mn<4+> doped fluoride fluorescent powder material | |
| CN1280864C (en) | Plasma display device | |
| CN1664051A (en) | Magnesia coated fluorescent powder and its coating method | |
| EP2915863A1 (en) | Silicate luminescent material and preparation method therefor | |
| CN101586026A (en) | A kind of PDP manufacture method of BAM blue colour fluorescent powder | |
| CN104271706A (en) | Core-shell structured silicate luminescent material and preparation method therefor | |
| CN101665689B (en) | Method for coating MgF2 film on surface of fluorescent powder | |
| CN115197690B (en) | Orange-red fluorescent powder and preparation method thereof | |
| CN100338715C (en) | Plasma display device and method for preparing phosphor | |
| CN102869749A (en) | Borate based red light emitting material and preparation method thereof | |
| CN104212443B (en) | The preparation method of short persistence zinc manganese silicate fluorescent material | |
| CN112592711B (en) | Far-red light fluorescent powder and preparation and modification methods thereof | |
| CN1664058A (en) | Process for preparing aluminate green fluorescent powder for plasma display device | |
| CN100473711C (en) | Phosphor, method for manufacturing the same and plasma display panel containing the same | |
| CN1294233C (en) | Process for preparing silicate green fluorescent powder | |
| CN100447298C (en) | Method for cladding titanium dioxide nano film on surface of zinc sulphide phosphor powder | |
| CN102337126B (en) | Preparation method of BAM (BaMgAl10O17) blue fluorescent powder for PDP (plasma display panel) | |
| CN101696356B (en) | Method for manufacturing borate green phosphor | |
| CN103409138A (en) | Preparation method of CNTs (Carbon Nano Tubes) used on PDP (Plasma Display Panel) and mixed with fluorescent powder | |
| CN104031641B (en) | Fluorescent material based on the aluminate fluorescent powder surface coating method of hydro-thermal reaction and preparation thereof | |
| CN1277898C (en) | Method for post-treatment of fluorescent materials | |
| CN1279140C (en) | Prepn process of blue aluminate phosphor |
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 |
Application publication date: 20050907 Assignee: Jiangsu Borui Photoelectric Co., Ltd. Assignor: Southeast University Contract record no.: 2010990000155 Denomination of invention: Silicon oxide coated fluorescent powder and its coating method Granted publication date: 20061129 License type: Exclusive License Record date: 20100330 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20061129 Termination date: 20200225 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |