CN1791702A - A method to encapsulate phosphor via chemical vapor deposition - Google Patents
A method to encapsulate phosphor via chemical vapor deposition Download PDFInfo
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- CN1791702A CN1791702A CN 200480013351 CN200480013351A CN1791702A CN 1791702 A CN1791702 A CN 1791702A CN 200480013351 CN200480013351 CN 200480013351 CN 200480013351 A CN200480013351 A CN 200480013351A CN 1791702 A CN1791702 A CN 1791702A
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- phosphorescent substance
- vuv
- phosphorescent
- phosphor
- europium
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Abstract
The maintenance characteristics of the phosphors used in VUV-excited devices such as plasma display panels can be improved by applying a coating of an aluminum oxyhydroxide compound by reacting vaporized trimethylaluminum with water vapor at a temperature of about 430 DEG C. or above. In particular, the maintenance of an europium-activated, calcium-substituted barium hexa-aluminate phosphor is significantly improved following exposure to a high intensity VUV flux.
Description
Cross reference with related application
The application requires all in the U.S. Provisional Application No.60/470 of application on May 15th, 2003,734 and 60/470,635 rights and interests.
Technical field
The present invention relates to be used for the method for packing of the phosphor particles of vacuum ultraviolet (VUV) (VUV)-excitation apparatus.Especially, the present invention relates to encapsulate phosphor is avoided moisture invasion and attack, VUV irradiation and Xe plasma bombardment with the protection phosphor particles method.
Background of invention
Conventional plasma display panel and other vacuum ultraviolet (VUV) (VUV)-excitation apparatus are filled with rare gas or rare gas (helium, neon, argon, xenon and krypton) mixture, by high-tension current they are excited and VUV scope below the 200nm wavelength in send uv-radiation.Adopt then this VUV radiation of sending excite various turning blue-, green-and the phosphorescent substance of ruddiness.These phosphorescent substances are with the different of those in being generally used for conventional luminescent lamp, and they are excited less than the high energy vacuum ultraviolet photon of 200nm by wavelength, and the 254nm's that the excitation energy of conventional luminescent lamp mainly is a mercuryvapour launches is more low-yield.Current, the most frequently used VUV excitation energy is from xenon or xenon-helium plasma, and it is launched in the zone of 147nm-173nm, and emmission spectrum depends on the concentration of xenon and the main assembly of gas accurately.Excite down at high pressure, generally have the xenon spectral line of emission and near the xenon excimer broadband emission the 173nm (excimer band emission) at 147nm place based on the plasma body of xenon.The huge difference of excitation energy has proposed new demand to the display panel that is used for VUV-and excites or the phosphorescent substance of lamp between vacuum ultraviolet (VUV) and the conventional shortwave fluorescence purposes.And then VUV-excites and the difference of conventional fluorescent apparatus production technique has also proposed new demand to phosphorescent substance.
Usually, be used for launching the phosphorescent substance that the VUV-of whole three kinds of colors (red, green and blue) excites and present some unfavorable performances, but be commonly used for the phosphorescent substance-Ba of blue emission body
1-
xEu
xMgAl
10O
17(0.01＜x＜0.20) or BAM problem maximum.Known this phosphorescent substance is in process of production because high temperature and humidity can be in variation aspect two in brightness and the color.For a long time after high strength xenon plasma body and VUV photon flux expose, this phosphorescent substance also can be in variation aspect two in brightness and the color.The mechanism of BAM degeneration (degradation) is the themes of a lot of researchs and is considered to relate to following variation: Eu
2+Be oxidized to Eu
3+, the change of the practical structures of aluminate phosphorus lattice and Eu
2+The motion that different positions is asked in lattice of exciting agent ion.Because gamut and blue phosphor component strength reduction, the useful life longevity of commercial plasma display panel is short as can not to make us accepting, and this causes the display panel integral color that undesirable Huang takes place moving.The measure the most relevant with this variation is the ratio of keeping intensity (I) and CIEy color dot, I/y.The strength degradation that degeneration produces and the rising of CIEy chromaticity coordinates cause the decline of I/y ratio jointly.
In recent years, attempted multiple different approaches to improve the retentivity of blue VUV-excitation photon.These approach comprise the sol-gel coating of broad-band gap metal oxide on the BAM phosphorescent substance, the thermal treatment of aluminate phosphorus and Neutral ammonium fluoride mixture, BAM phosphorescent substance chain polyphosphate based on solution applies, basic metal, alkaline-earth metal or zinc are substituted onto in the stoichiometry of BAM, and preparation BAM-six barium aluminate (0.82BaO6Al
2O
3) sosoloid of phase, it demonstrates improved colour stability and retentivity, but has unfavorable color dot.In addition, studied novel phosphorescent substance, as (La with improved preserving property
1-x-y-zTm
xLi
ySr
z) PO
4, Ba
1-aEu
aMgAl
6O
11, CaMgSi
2O
6: Eu
2+And CaAl
2O
4: Eu
2+
Though the improvement that much demonstrates color and strength stability aspect in these phosphorescent substances or the phosphor composite does not all confirm it is feasible alternative as yet.Thereby, still there is business demand in the blue-light-emitting VUV-excitation phosphor of degenerative character with reduction.Especially, wish that following performance is arranged: the high relative percentage retentivity of the heat of improved life-span and acceleration in improved colour stability, the display panel working process in darker blueness, the display panel manufacturing processed, wet, xenon plasma body and high-strength V UV photon flux test back I/y.
Summary of the invention
Recent findings can be used as acceptable blue-light-emitting phosphorescent substance and the degeneration that presented by the BAM phosphorescent substance through six barium aluminates (CBAL) phosphorescent substance that europium excites, calcium replaces in the VUV-excitation apparatus.In the past,, the CBAL phosphorescent substance was described as conventional fluorescent phosphor in 187, used, be not used for the VUV-excitation apparatus but be described up to now with mercury gas discharge in U.S. Patent No. 4,827.Preferably, the CBAL phosphorescent substance has formula Ba
1.29-x-yCa
xEu
yAl
12O
19.29The composition that characterizes, wherein 0＜x＜0.25 and 0.01＜y＜0.20.
Excite down at VUV, the CBAL phosphorescent substance demonstrates the blue emission peak darker than BAM phosphorescent substance, but only is the 80-85% that is purchased the initial strength of BAM phosphorescent substance.Yet when being exposed to hot and humid condition, the CBAL phosphorescent substance demonstrates on color dot and is in close proximity to zero green moving and minimum loss of strength.And then when the high-strength V UV photon flux that is exposed to as accelerated weathering test, the CBAL phosphorescent substance demonstrates less than the strength degradation of commercial BAM phosphorescent substance 1/2 and is in close proximity to zero gamut.
We find, by aluminium hydroxide (aluminium oxyhydroxide) coating being administered on the one phosphor particles in fluidized-bed reactor via the chemical vapor deposition (CVD) technology, some preserving property of CBAL phosphorescent substance and other VUV phosphorescent substance can be significantly improved.This novel method has been used the trimethyl aluminium (TMA) of vaporization and the reaction between the water vapour.In the past, in U.S. Patent No. 5,080,928 and 5,220,243 for example, the reaction of TMA/ water was described as being used to apply the electroluminescent phosphor that is mainly zinc sulfide-based.Yet, in the method for the invention, under the much higher temperature of in than prior art, point out 300 ℃ or lower temperature, about 430 ℃ or higher, implement the reaction of TMA/ water.Can not produce in the VUV-excitation phosphor and make the VUV phosphorescent substance avoid any remarkable provide protection of moisture invasion and attack being generally used under 180 ℃ of ZnS electroluminescent phosphor reactive applications with TMA/ water.The coating of cold condition deposit it is believed that density is not enough to prevent the infiltration of water molecules.Thereby, need higher temperature condition to apply improved preserving property.
The accompanying drawing summary
This figure has illustrated the equipment that is used for the inventive method.
Detailed Description Of The Invention
In order to understand better the present invention, and other target, advantage and ability, please refer to the following discloses content, and in conjunction with appending claims and above-mentioned accompanying drawing.
Chemical vapour deposition (CVD) prevents that the method for packing that phosphor particles is degenerated from having obtained open in many employing fluidized-bed reactors. Yet plasma display panel (PDP) is difficult to fluidisation with small size (3-5 micron, D50 size) blue phosphor such as BAM and the CBAL utmost point, and this is because its adhesiveness. Also has the Eu in these phosphors2+Exciting agent is very easily oxidized under oxidation environment. Method of the present invention be can be used for encapsulating to oxidation-sensitive with other the hydrolysis process of VUV-excitation phosphor. Steam not only is used for other reaction reaction also helping the fluidisation of fine size phosphor particles to form coating. The method applied chemistry gas phase deposition technology single phosphor powder particle deposited through the hydrolysis the trimethyl aluminium compound film. Although some is difficult to the composition of the trimethyl aluminium compound through being hydrolyzed determine, can describe it as aluminium hydroxide to a great extent. In coating procedure, described Particles Suspension in fluid bed and under about 430 ℃ or higher bed temperature, is exposed the trimethyl aluminium precursor of vaporizing in the inert carrier gas. Simultaneously, making inert gas, generally is nitrogen via the water foam maker of heating, and steam is written in the reactor. Next, the hydrone of gaseous state and trimethyl aluminium steam reaction form continuous coated on the phosphor powder surface. Have been found that the coating of hot conditions deposit on the PDP phosphor significantly improved the moisture resistance properties of phosphor. For the effect of demonstration coating, with this pyrohydrolysis coating processes encapsulate phosphor, then test under various conditions.
Apply operation
All coated test are all carried out in the quartz tube reactor of internal diameter 14cm, length 152cm.With reference to the accompanying drawings, for each operating process, the phosphorescent substance 60 of 4.0kg is packed in the reactor 16.At first, thus the bottom of the inert nitrogen fluidizing agent being introduced reactor 16 with 15 liters/minute flow velocity makes the phosphor particles fluidisation.This phosphor particles is suspended in the fluidized-bed reactor by nitrogen, is suspended into the bed height of about 100cm.Then, start the circulation of helping phosphor particles in the reactor through the vibromixer 19 of top insertion reaction device 16 with the speed of 60 cycle per minute clocks.Utilize external furnace 20 with fluidized-bed reactor heating and when being maintained at about 430 ℃, in this reactor, place two thermopairs to monitor this temperature distribution.A middle part that is arranged in bed is used in coating processes controlling reactor temperature at ± 5 ℃.Another is positioned at 1 inch place, divider 33 tops, and divider 33 is positioned on the bottom of reactor.When temperature of reactor during near 430 ℃, starting TMA pre-treatment step.Nitrogen carrier gas 11 is with 8.0 liters of/minute trimethyl aluminium foam makers 12 of flowing through.The temperature that the TMA foam maker is remained on 34 ℃ is to keep the TMA vapour pressure constant.Nitrogen gas stream 13 and 15.0 liters/minute the nitrogen gas stream gasification stream 5 that will contain the trimethyl aluminium precursor of vaporization mix and make the base portion of its inflow fluidized-bed reactor.The trimethyl aluminium precursor vapor of this dilution is carried through the metal sintering divider 33 that is positioned at the reaction tubes below and is used for supporting the phosphor particles bed.After saturated 1 minute, water vapor is transported in the reactor via the 3rd nitrogen gas stream 23 by the TMA precursor on the phosphor powder surface with 14 liters/minute flow velocitys.Via water-filled foam maker 22 supplying nitrogen carrier gas streams 17, described foam maker 22 remains on 70 ℃ temperature.The mixture 23 of water vapor and nitrogen via the pore inflow reactor of circle distribution on the tubular shaft 7 of a series of vibromixers 19 that are positioned at vibration disc 3 tops with the beginning coating procedure.Make to apply and react the hydrolysis TMA coating of carrying out until producing aequum.
Designing the test of hot humidity and accelerated deterioration produces and operation to simulate actual PDP plate.By adopting Perkin-Elmer LS-50B spectrometer measurement emmission spectrum and making it carry out the brightness that quantification treatment has obtained hot humidity and accelerated weathering test front and back with respect to standard reference BAM phosphorescent substance emmission spectrum.With this spectrum derive the peak wavelength at maximum strength place and adopt from this spectroscopic data known and accepted based on X, Y, Z-three look curve's equation calculate y coordinate colour.Excitaton source is that the xenon exciter lamp (from Resonance, Ltd., Barrie, Ontario, the XeCM-L of Canada) that is purchased is used for illuminating the powder plate, air is got rid of penetrated outside the path at VUV simultaneously.Also phosphorescent substance can be sneaked into lotion, be coated on aluminum oxide chip or " slide glass ", and measure in this mode.
Hot wet test comprises the phosphorescent substance sample is exposed 2 hours to warm, water saturated airflow at 425 ℃.Accelerated weathering test comprises to high strength xenon plasma body and the exposure of VUV photon flux.Adopt superpower noble gas discharge chamber to carry out accelerated weathering test.This chamber is by the 5cm I.D.Pyrex of 100cm
TMLoop pipe is formed, and originally it be evacuated to 10
-6The xenon stream that has about 5 milli-torrs behind the holder ear.After applying about 280 watts power input with 450KHZ, obtained inducing the coupling discharge from the RF power supply.According to estimates, on sample surfaces, there is about 90 milliwatts/cm
2The VUV radiation of 147nm. do not have tangible quasi-molecule atomic emissions under these conditions and take place.After exposing a selected amount of time, by the brightness of above-mentioned measure sample to xenon gaseous discharge.
Experimental example 1
CBAL (cCBAL) sample that preparation CBAL and pyrohydrolysis TMA-apply is also collected their emmission spectrum.Make sample by the above-mentioned degradation experiment that stands then.Pyrohydrolysis TMA coating use the remarkable preserving property that improves the CBAL phosphorescent substance.The initial optical emitting result with CBAL that degenerates and cCBAL phosphorescent substance is provided at (with making comparisons as correlated standard BAM phosphorescent substance) in the following table 1.Term " TH " refers to the hot and humid exposure of warp-wise and the sample of degenerating; Term " X " refers to warp-wise high strength xenon plasma body and the VUV photon flux exposes and the sample of degeneration; Term " THX " refers to the hot and humid exposure of warp-wise and then exposes and the sample of degeneration to high strength xenon plasma body and VUV photon flux.Measurement is with respect to the intensity of the PDP BAM phosphorescent substance of standard blue light-emitting.
Table 1
| Powder plate data | Lotion slide glass data | |||||
| BAM (contrast) | CBAL | cCBAL | BAM (contrast) | CBAL | cCBAL | |
| Intensity (initially) | 96％ | 76％ | 68％ | 104％ | 84％ | 79％ |
| Peak value λ (initially) | 446 nm | 439 nm | 439 nm | 446 nm | 439 nm | 439 nm |
| Y value (initially) | 0.0465 | 0.0568 | 0.0553 | 0.0466 | 0.0518 | 0.0517 |
| Intensity (TH) | 87％ | 74％ | 69％ | 96％ | 82％ | 79％ |
| Peak value λ (TH) | 456nm | 439 nm | 439 nm | 456 nm | 439 nm | 439 nm |
| Y value (TH) | 0.0803 | 0.0571 | 0.0566 | 0.0771 | 0.0527 | 0.0542 |
| ％I/y (TH) | 52％ | 96％ | 98％ | 56％ | 96％ | 95％ |
| Intensity (X) | 57％ | 42％ | 49％ | 76％ | 61％ | 66％ |
| Peak value λ (X) | 446 nm | 439 nm | 439 nm | 446 nm | 439 nm | 439 nm |
| Y value (X) | 0.0527 | 0.0625 | 0.0608 | 0.0504 | 0.0565 | 0.0563 |
| ％I/y (X) | 53％ | 50％ | 65％ | 68％ | 66％ | 76％ |
| Intensity (THX) | 52％ | 47％ | 49％ | 64％ | 60％ | 65％ |
| Peak value λ (THX) | 454nm | 439 nm | 439 nm | 454 nm | 439 nm | 439 nm |
| Y value (THX) | 0.0901 | 0.0642 | 0.0633 | 0.0905 | 0.0596 | 0.0602 |
| ％I/y (THX) | 28％ | 54％ | 63％ | 32％ | 62％ | 70％ |
Similar from the degeneration result that powder and lotion sample obtain.The peak wavelength at maximum strength place does not change for CBAL or cCBAL, and the BAM comparative sample demonstrates big gamut after hot wet test.The correlated original intensity of BAM is more much higher than the original intensity of CBAL and cCBAL sample, and after thermotropism wet test and high strength Xe plasma body and the exposure of VUV photon flux, all samples all have suitable brightness.Wet and Xe plasma body test (THX) afterwards in heat, the retentivity of the I/y ratio (%I/y) of CBAL sample is higher than BAM contrast (54%vs.28% and 62%vs.32%) far away, and the retentivity of the CBAL (cCBAL) through applying has further improvement (63%vs.54% and 70%vs.62%) .cCBAL material to demonstrate significantly improved retentivity after independent high strength Xe plasma body and VUV photon flux exposure (X) than uncoated CBAL.
Embodiment 2
Zinc silicate (the Zn that manganese excites
2SiO
4: Mn) be the high-level efficiency green emission phosphorescent substance of plasma display panel.This phosphorescent substance is highly stable in PDP plate production process.After hot and humid exposure, do not observing tangible brightness variation and gamut.Yet, under ion bombardment and plasma body VUV irradiation, the obvious variation of phosphorescent substance brightness.For improving the brightness retentivity, the method according to this invention applies Zn with the aluminium hydroxide coating
2SiO
4: Mn phosphorescent substance (OSRAMSYLVANIA 9310 types).Effect for hydrolysis TMA coating under the contrast accelerated weathering test condition encapsulates phosphor powder under low (180 ℃) and high (430 ℃) temperature of reaction.Phosphorescent substance uncoated and that applied mixed with lotion and tackiness agent burnt (BBO).Measure original intensity (behind the BBO) and final brightness (exposing the back) and calculate retentivity (the finally ratio of brightness/original intensity) to high strength Xe plasma body and VUV photon flux.The result of these measurements is provided in the table 2.
Table 2
| Sample | Elemental height, % | Final brightness, % | Retentivity, % |
| Uncoated | 100 | 74.8 | 74.8 |
| Apply down at 180 ℃ | 84.8 | 62.8 | 74.0 |
| Apply down at 430 ℃ | 80.7 | 69.5 | 86.0 |
Based on the data shown in the table 2, during TMA hydrolysis reaction encapsulate phosphor under adopting 180 ℃, do not observe the raising of brightness retentivity.Yet when under 430 ℃ temperature hydrolysis TMA being coated with when being deposited to phosphor surface, the brightness retentivity improves significantly to 86.0% from 74.8%.
Shown and described the current preferred embodiment of the invention of thinking that under the situation that does not deviate from the scope of the invention that claims determine, can carry out various variations and improvement to it, this will be apparent to those skilled in the art.
Claims (10)
1, the method for encapsulate phosphor comprises:
(a) fluidisation phosphor particles in fluidized-bed reactor;
(b) described particle is exposed to the trimethyl aluminium of vaporization;
(c) under about 430 ℃ or higher temperature, make water vapor and trimethyl aluminium reaction, thereby on phosphor particles, form the coating of hydrolysis trimethyl aluminium compound.
2, the phosphor particles that the process of claim 1 wherein comprises the six barium aluminate phosphorescent substances that europium-excite, calcium replace.
3, the phosphor particles that the process of claim 1 wherein comprises the zinc silicate phosphorescent substance that manganese excites.
4, the method for claim 2, wherein be reflected at about 430 ℃ of generations.
5, the method for claim 3, wherein be reflected at about 430 ℃ of generations.
6, the method for claim 2, the composition of the six barium aluminate phosphorescent substances that wherein europium excites, calcium replaces is by formula Ba
1.29-x-yCa
xEu
yAl
12O
19.29Expression, wherein 0＜x＜0.25 and 0.01＜y＜0.20.
7, the method for claim 6, wherein be reflected at about 430 ℃ of generations.
8, according to the phosphorescent substance of the method for claim 1 encapsulation, the six barium aluminate phosphorescent substances that phosphorescent substance wherein is an europium-excite, calcium replaces.
9, the phosphorescent substance of claim 8, the composition of the six barium aluminate phosphorescent substances that wherein europium excites, calcium replaces is by formula Ba
1.29-x-yCa
xEu
yAl
12O
19.29Expression, wherein 0＜x＜0.25 and 0.01＜y＜0.20.
10, according to the phosphorescent substance of the method for claim 1 encapsulation, phosphorescent substance wherein is the zinc silicate phosphorescent substance that manganese excites.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US47063503P | 2003-05-15 | 2003-05-15 | |
| US60/470,635 | 2003-05-15 | ||
| US60/470,734 | 2003-05-15 |
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| Publication Number | Publication Date |
|---|---|
| CN1791702A true CN1791702A (en) | 2006-06-21 |
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ID=36785135
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|---|---|---|---|
| CN 200480013351 Pending CN1791702A (en) | 2003-05-15 | 2004-05-13 | A method to encapsulate phosphor via chemical vapor deposition |
| CN200480013187A Active CN100583352C (en) | 2003-05-15 | 2004-05-13 | VUV-excited device with blue-emitting organic light-emitting material |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107267256A (en) * | 2017-06-28 | 2017-10-20 | 常州蓝旗亚纺织品有限公司 | A kind of preparation method of lubricating oil nanometer detersive |
| CN107312521A (en) * | 2017-06-07 | 2017-11-03 | 常州苏达欧包装材料有限公司 | A kind of preparation method of luminescent powder |
| CN107718180A (en) * | 2017-09-16 | 2018-02-23 | 常州海瑞纺织品有限公司 | A kind of poplar plywood and preparation method thereof |
| CN112159213A (en) * | 2020-10-29 | 2021-01-01 | 贵州赛义光电科技有限公司 | Zero-light-decay luminescent ceramic and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3670194A (en) * | 1971-01-26 | 1972-06-13 | Westinghouse Electric Corp | Color-corrected high-pressure mercury-vapor lamp |
| EP0241848B1 (en) * | 1986-04-16 | 1990-03-14 | Kabushiki Kaisha Toshiba | Phosphor and fluorescent lamp using the same |
-
2004
- 2004-05-13 CN CN 200480013351 patent/CN1791702A/en active Pending
- 2004-05-13 CN CN200480013187A patent/CN100583352C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107312521A (en) * | 2017-06-07 | 2017-11-03 | 常州苏达欧包装材料有限公司 | A kind of preparation method of luminescent powder |
| CN107267256A (en) * | 2017-06-28 | 2017-10-20 | 常州蓝旗亚纺织品有限公司 | A kind of preparation method of lubricating oil nanometer detersive |
| CN107718180A (en) * | 2017-09-16 | 2018-02-23 | 常州海瑞纺织品有限公司 | A kind of poplar plywood and preparation method thereof |
| CN112159213A (en) * | 2020-10-29 | 2021-01-01 | 贵州赛义光电科技有限公司 | Zero-light-decay luminescent ceramic and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1788326A (en) | 2006-06-14 |
| CN100583352C (en) | 2010-01-20 |
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