CN101581808A - Light-conversion nano-film for PDP display, and preparation method thereof - Google Patents

Light-conversion nano-film for PDP display, and preparation method thereof Download PDF

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Publication number
CN101581808A
CN101581808A CNA2009100331200A CN200910033120A CN101581808A CN 101581808 A CN101581808 A CN 101581808A CN A2009100331200 A CNA2009100331200 A CN A2009100331200A CN 200910033120 A CN200910033120 A CN 200910033120A CN 101581808 A CN101581808 A CN 101581808A
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film
light
orange
preparation
conversion nano
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CN101581808B (en
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颜悦
张官理
张小华
潘耀南
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NANJING JUCHENG TECHNOLOGY Co Ltd
Beijing Institute of Aeronautical Materials China Aviation Industry No 1 Group Corp
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NANJING JUCHENG TECHNOLOGY Co Ltd
Beijing Institute of Aeronautical Materials China Aviation Industry No 1 Group Corp
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Abstract

The invention provides a light-conversion nano-film for PDP display, and a preparation method thereof. The light-conversion nano-film for PDP display comprises a flexible organic base material layer, an intermediate transition layer and an upper conversion luminescent layer, wherein the intermediate transition layer is arranged on the flexible organic base material layer; the upper conversion luminescent layer is arranged on the intermediate transition layer; and the upper conversion luminescent layer is a composite material prepared from 40CdF2 . 60BaF2 . 1.6Er2O3 compounds doped with orange-light absorption dye. The preparation method comprises the following steps: subjecting one surface of PET to hardening treatment and providing the surface subjected to the hardening treatment with 1 to 20 transition layers; preparing the 40CdF2 . 60BaF2 . 1.6Er2O3 compounds doped and mixed with the orange-light absorption dye into a target, or preparing the 40CdF2 . 60BaF2 . 1.6Er2O3 compounds and the orange-light absorption dye into targets respectively; and utilizing target materials prepared in a second step to coat the transition layers of the flexible organic base material prepared in a first step with a film in a magnetron sputtering furnace. The film layer can absorb visible light between 580 and 600 nm and convert the visible light into ultraviolet light between 200 and 380 nm.

Description

Be used for light-conversion nano-film of PDP demonstration and preparation method thereof
Technical field
The present invention relates to a kind of PDP and show, belong to display material and make the field, relate in particular to the field of nano material preparation of the light conversion that contains rare earth element with light conversion film and preparation method thereof.
Background technology
The PDP displaying principle utilizes the making alive method to make it emit ultraviolet ray for the gas to being full of between the upper and lower glass substrate, and ultraviolet ray shines the fluorescent powder on glass tube surface and emits visible rays.The ultraviolet ray that utilizes gas discharge to produce shines fluorescent powder and there are countless small spacers in luminous flat-panel monitor between electroded two glass substrates, so can keep certain spacing between each adjacent cells, and shape in an overlapping.Between two glass substrates, be full of sealing gas (Ne, Xe), be used for discharge.
Can produce the orange-colored light of 592nm when the Ne gas discharge, the appearance of orange-colored light has destroyed colour purity, therefore must eliminate the Ne-cut of common name that Here it is.
Present method in common is the orange-colored light that the mode of employing gluing absorbs 592nm, the method has had a strong impact on the transmittance of PDP colour TV, the loss of transmittance surpasses 20%, PDP screened film transmittance one of the main reasons between 40%-50% all at present that Here it is.
One big characteristics of rare earth metal are exactly photoluminescence, and colour TV is exactly to utilize these characteristics of rare earth metal to absorb ultraviolet light with fluorescent powder and illumination lamp phosphor, sends visible lights such as red, green, blue.The glimmering conversion agent of agricultural film rare-earth can be converted to plant with the visible light to the harmful ultraviolet light of plant production and other wavelength and carry out near blue light (440 nanometers) and near the ruddiness (660 nanometers) that photosynthesis needs.
The rare earth element not only can be shorter than wavelength the ultraviolet ray of 400nm, and X ray etc. convert the visible light in 400～760mm scope to, also can change infrared ray into visible light.Thisly make the shorten conversion of (promptly strengthening luminous energy) of wavelength be referred to as " going up conversion ".Aspect civilian, can utilize " going up conversion " function of rare earth material to be that the infrared heat energy that bulb produces converts visible light to tungsten, thereby to put forward the light luminescence efficiency greatly.Aspect military, utilize rare earth " to go up conversion ".Material can change infrared ray into visible light, thereby visits clear target azimuth etc.Having this respect materials with function has: be mixed with the BaYF5 of Yb3+Er3+ and be mixed with Yb3+ and the LaF3 of Er3+ and be mixed with the GdF3 etc. of Yb3+ and Tm3+.
Summary of the invention
Shield the low shortcoming of integral light-transmitting rate of filter coating for the PDP that solves the prior art existence, the invention provides light-conversion nano-film of a kind of PDP of being used for demonstration and preparation method thereof, the brightness that the light-conversion nano-film that is used for the PDP demonstration that adopts method of the present invention to prepare can effectively improve the PDP display.
Technical scheme of the present invention is: a kind of light-conversion nano-film that is used for the PDP demonstration, described light-conversion nano-film comprises flexible organic ground bed of material, intermediate layer, up-conversion luminescence layer, flexible organic ground bed of material is provided with intermediate layer, intermediate layer is provided with the up-conversion luminescence layer, and the up-conversion luminescence layer is CdF 2, BaF 2, Er 2O 3Complex 40CdF 260BaF 21.6Er 2O 3With the compound substance of making after the doping of orange-colored light absorbing dye.The thickness of light-conversion nano-film is between 10nm～30nm.The selection of concrete thickness will be according to the structure of PDP demonstration, the factors such as ratio of Ne gas, and optimum value is the 592nm orange-colored light that just in time absorbs conversion Ne fully.The organic ground bed of material of described flexibility is a polyethylene terephthalate materials, is called for short the PET material, and can satisfy the flat-panel monitor request for utilization: thickness is 0.1mm～0.15mm, and transmittance is greater than 98%, and condensation rate is less than 5%.The purpose of selecting flexible organic group bottom material is to twine plated film continuously in order to realize, can realize large-scale production, low-cost high production easily like this.To the requirement of PET material mainly is that weatherability, good corrosion resistance, thermal expansivity are little, and the density height of material can not chap, and does cure process in the one side of this base material, and the skin hardness after the processing requires to reach the color TV enterprises standard.Described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.The number of plies of intermediate layer is 1～20, and intermediate layer can be TiO 2Transition beds such as layer, Ag layer, metallic crystal anti-reflection layer, ITO layer.
The described preparation method who is used for the light-conversion nano-film of PDP demonstration comprises the steps:
The first step prepares flexible organic bottom material: the one side of polyethylene terephthalate materials is done cure process, make the skin hardness after the processing meet the ASTM-D-1044 standard, be provided with 1～20 layer of transition bed on that good face of cure process;
Second step, preparation target: with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are prepared into target by 1: 50 mixing and doping or with 40CdF 260BaF 21.6Er 2O 3Complex, orange-colored light absorbing dye are prepared into target respectively;
The 3rd step, magnetron sputtering: utilize the target material of second step preparation, in the magnetron sputtering stove, vacuumize greater than 10 earlier -3Behind the Pa, charge into and keep behind the Ar gas operating air pressure 5 * 10 -2Pa, plated film on the transition bed of flexible organic bottom material that the first step prepares just prepares the up-conversion luminescence layer, and rate of sedimentation is controlled to be 0.1nm/s, and the thickness of control light-conversion nano-film is 10nm～30nm.
In second step, press 40CdF 260BaF 21.6Er 2O 3Complex and 1: 50 ratio of orange-colored light absorbing dye mass ratio are got orange-colored light absorbing dye and 40CdF 260BaF 21.6Er 2O 3Put in orange-colored light absorbing dye and deionized water quality and put into deionized water than 1: 4 ratio, behind the ultrasonic dispersion 15min of frequency 80KHz power 50W, be heated to boiling constant temperature 30min, filter and clean, put into crucible and heat up with the speed of 2 ℃/min, be heated to 500 ℃ and be incubated 3h, obtain 40CdF behind the cooling forming at muffle furnace 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are pressed the target of mass ratio mixing and doping preparation in 1: 50.
Second the step in, the preparation target material concrete grammar also can for: with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are made target material respectively, and then carry out the composition target magnetron sputtering.
In second step, 40CdF 260BaF 21.6Er 2O 3The concrete grammar of the preparation of complex is: with CdF 2, BaF 2, Er 2O 340: 60: 1.6 in molar ratio ratio mixes after grinding, and mix powder is put into sintering furnace is heated to 1000 ℃ of sintering 10min after annealing obtains complex 40CdF 260BaF 21.6Er 2O 3Experimental data shows: CdF 2BaF 2Er 2O 3Ratio between 40: 60: 2～40: 60: 0.5, can realize the light output of 200nm～380nm, it is slightly variant to absorb conversion spectrum.This experiment selects for use 40: 60: 1.6 ratio near the absorption spectrum of PDP display fluorescent powder.
Described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.The light-conversion nano-film that the described PDP of being used for shows is used to prepare light-filtering screened film.
Beneficial effect: the light conversion film that the present invention is prepared, utilized the last transfer principle of rare earth element, the radiant light of absorption of N e in the 580nm-600nm zone, be converted to wavelength and be the ultraviolet light between the 200nm-380nm, strengthen the exposure intensity of ultraviolet light, so not only solve the Ne-cut problem, strengthened the exposure intensity of ultraviolet light simultaneously, improved the brightness of PDP.Integral light-transmitting rate with the PDP shielding filter coating of this technology preparation can reach 60%-70%, improves 20% than the brightness of existing product.
Description of drawings
Fig. 1 is the cross-sectional view that is used for the light-conversion nano-film of PDP demonstration of the present invention.
1 is light conversion layer among the figure, and 2 is transition bed, and 3 is flexible organic ground bed of material.
Embodiment
A kind of light-conversion nano-film that is used for the PDP demonstration, described light-conversion nano-film comprises flexible organic ground bed of material, intermediate layer, up-conversion luminescence layer, flexible organic ground bed of material is provided with intermediate layer, and intermediate layer is provided with the up-conversion luminescence layer, and the up-conversion luminescence layer is 40CdF 260BaF 21.6Er 2O 3The compound substance that complex and orange-colored light absorbing dye are made after mixing.The thickness of light-conversion nano-film is between 10nm～30nm.The selection of concrete thickness will be according to the structure of PDP demonstration, the factors such as ratio of Ne gas, and optimum value is the 592nm orange-colored light that just in time absorbs conversion Ne fully.The organic ground bed of material of described flexibility is a polyethylene terephthalate, is called for short PET, and can satisfy the flat-panel monitor request for utilization: thickness is 0.1mm～0.15mm, and transmittance is greater than 98%, and condensation rate is less than 5%.The purpose of selecting flexible organic group bottom material is to twine plated film continuously in order to realize, can realize large-scale production, low-cost high production easily like this.To the requirement of PET material mainly is that weatherability, good corrosion resistance, thermal expansivity are little, and the density height of material can not chap, and does cure process in the one side of this base material, and the skin hardness after the processing requires to reach the color TV enterprises standard.Described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.The number of plies of intermediate layer is 1～20, and intermediate layer can be TiO 2Layer, Ag layer, metallic crystal anti-reflection layer, ITO layer etc.
A kind of preparation method who is used for the light-conversion nano-film of PDP demonstration comprises the steps:
The first step prepares flexible organic bottom material: the one side of polyethylene terephthalate materials is done cure process, make the skin hardness after the processing meet the ASTM-D-1044 standard, be provided with 1～20 layer of transition bed on that good face of cure process;
Second step, preparation target: with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are prepared into target by 1: 50 mixing and doping of mass ratio or with 40CdF 260BaF 21.6Er 2O 3Complex, orange-colored light absorbing dye are prepared into target respectively;
The 3rd step, magnetron sputtering: utilize the target material of second step preparation, in the magnetron sputtering stove, vacuumize greater than 10 earlier -3Behind the Pa, charge into and keep behind the Ar gas operating air pressure 5 * 10 -2Pa, plated film on the transition bed of flexible organic bottom material that the first step prepares just prepares the up-conversion luminescence layer, and rate of sedimentation is controlled to be 0.1nm/s, and the thickness of control light-conversion nano-film is 10nm～30nm.
In second step, 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye by the concrete grammar that 1: 50 mixing and doping of mass ratio prepares target are: press 40CdF 260BaF 21.6Er 2O 3Complex and 1: 50 ratio of orange-colored light absorbing dye mass ratio are got orange-colored light absorbing dye and 40CdF 260BaF 21.6Er 2O 3Put in orange-colored light absorbing dye and deionized water quality and put into deionized water than 1: 4 ratio, behind the ultrasonic dispersion 15min, be heated to boiling constant temperature 30min, filter and clean, put into crucible and heat up with the speed of 2 ℃/min, be heated to 500 ℃ and be incubated 3h, obtain 40CdF behind the cooling forming at muffle furnace 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are pressed the target of mass ratio mixing and doping preparation in 1: 50.
Second the step in, the preparation target material concrete grammar also can for: with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are pressed into target material respectively, and then carry out the composition target magnetron sputtering.
In second step, 40CdF 260BaF 21.6Er 2O 3The concrete grammar of the preparation of complex is: with CdF 2, BaF 2, Er 2O 340: 60: 1.6 in molar ratio ratio mixes after grinding, and mix powder is put into sintering furnace is heated to 1000 ℃ of sintering 10min after annealing obtains complex 40CdF 260BaF 21.6Er 2O 3
Described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.The light-conversion nano-film that the described PDP of being used for shows is used to prepare light-filtering screened film.
Embodiment 1
A kind of preparation method who is used for the light-conversion nano-film of PDP demonstration comprises the steps:
The first step prepares flexible organic bottom material: the one side of polyethylene terephthalate materials is done cure process, make the skin hardness after the processing meet the ASTM-D-1044 standard, be provided with TiO on that good face of cure process 2Transition beds such as layer, Ag layer, metallic crystal anti-reflection layer, ITO layer;
Second step, preparation target: with CdF 2, BaF 2, Er 2O 340: 60: 1.6 in molar ratio ratio mixes after grinding, and mix powder is put into sintering furnace was heated to 1000 ℃ of sintering 10 minutes after annealing obtains complex 40CdF 260BaF 21.6Er 2O 3Weigh the 40CdF of 7.5g orange-colored light absorbing dye and 0.15g 260BaF 21.6Er 2O 3The beaker of 100mL is put in the up-conversion luminescence agent, put into the 30mL deionized water, behind the ultrasonic dispersion 15min, be heated to boiling constant temperature 30min, filter and clean, put into crucible and heat up with the speed of 2 ℃/min, be heated to 500 ℃ and be incubated 3h, obtain 1: 50 doping orange-colored light of up-conversion luminescence agent absorbing dye target behind the cooling forming at muffle furnace;
The 3rd step, magnetron sputtering: utilize the target of second step preparation, in the magnetron sputtering stove, vacuumize greater than 10 earlier -3Behind the Pa, charge into and keep behind the Ar gas operating air pressure 5 * 10 -2Pa, plated film on the transition bed of flexible organic bottom material that the first step prepares, rate of sedimentation is controlled to be 0.1nm/s, and the thickness of control light-conversion nano-film is 10nm～30nm.
Embodiment 2
A kind of preparation method who is used for the light-conversion nano-film of PDP demonstration comprises the steps:
The first step prepares flexible organic bottom material: the one side of polyethylene terephthalate materials is done cure process, make the skin hardness after the processing meet the ASTM-D-1044 standard, be provided with TiO on that good face of cure process 2Transition beds such as layer, Ag layer, metallic crystal anti-reflection layer, ITO layer;
Second step, preparation target: with CdF 2, BaF 2, Er 2O 340: 60: 1.6 in molar ratio ratio mixes after grinding, and mix powder is put into sintering furnace was heated to 1000 ℃ of sintering 10 minutes after annealing obtains complex 40CdF 260BaF 21.6Er 2O 3, with this up-conversion luminescence agent 40CdF 260BaF 21.6Er 2O 3Be pressed into the rectangle target respectively with tetra-tert tetraazatetradecane porphyrin cobalt;
The 3rd step, magnetron sputtering: utilize the target material of second step preparation, in the magnetron sputtering stove, vacuumize greater than 10 earlier -3Behind the Pa, charge into and keep behind the Ar gas operating air pressure 5 * 10 -2Pa, plated film on the transition bed of flexible organic bottom material that the first step prepares, 40CdF 260BaF 21.6Er 2O 3Two targets of complex and tetra-tert tetraazatetradecane porphyrin cobalt adopt different rate of sedimentation, and controlling its mass ratio is 1: 50, and the thickness of control light-conversion nano-film is 10nm～30nm.
The integral light-transmitting rate of the PDP shielding filter coating of the light-conversion nano-film preparation of employing present embodiment can reach 60%-70%.
Embodiment 3
Change the tetra-tert tetraazatetradecane porphyrin cobalt in embodiment 1 and 2 into tetra-tert tetraazatetradecane porphyrin lead.
Embodiment 4
Change the tetra-tert tetraazatetradecane porphyrin cobalt in embodiment 1 and 2 into ethyl violet.

Claims (10)

1, a kind of light-conversion nano-film that is used for the PDP demonstration, it is characterized in that, described light-conversion nano-film comprises flexible organic ground bed of material, intermediate layer, up-conversion luminescence layer, flexible organic ground bed of material is provided with intermediate layer, intermediate layer is provided with the up-conversion luminescence layer, and the up-conversion luminescence layer is complex 40CdF 260BaF 21.6Er 2O 3With the compound substance of making after the doping of orange-colored light absorbing dye.
2. the light-conversion nano-film that is used for the PDP demonstration as claimed in claim 1 is characterized in that the thickness of described light-conversion nano-film is between 10nm～30nm.
3. the light-conversion nano-film that is used for the PDP demonstration as claimed in claim 1 is characterized in that the organic ground bed of material of described flexibility is a polyethylene terephthalate, and thickness is 0.1mm～0.15mm, and transmittance is greater than 98%, and condensation rate is less than 5%.
4. the light-conversion nano-film that is used for the PDP demonstration as claimed in claim 1 is characterized in that described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.
5. the light-conversion nano-film that is used for the PDP demonstration as claimed in claim 1 is characterized in that the number of plies of intermediate layer is 1～20.
6. the preparation method who is used for the light-conversion nano-film of PDP demonstration as claimed in claim 1 is characterized in that, comprises the steps:
The first step prepares flexible organic bottom material: the one side of polyethylene terephthalate materials is done cure process, make the skin hardness after the processing meet the ASTM-D-1044 standard, be provided with 1～20 layer of transition bed on that good face of cure process;
Second step, preparation target: with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are prepared into target by 1: 50 mixing and doping of mass ratio or with 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are prepared into target respectively;
The 3rd step, magnetron sputtering: utilize the target material of second step preparation, in the magnetron sputtering stove, vacuumize greater than 10 earlier -3Behind the Pa, charge into and keep behind the Ar gas operating air pressure 5 * 10 -2Pa, plated film on the transition bed of flexible organic bottom material that the first step prepares just prepares the up-conversion luminescence layer, and rate of sedimentation is controlled to be 0.1nm/s, and the thickness of control light-conversion nano-film is 10nm～30nm.
7. the preparation method who is used for the light-conversion nano-film of PDP demonstration as claimed in claim 6 is characterized in that, in second step, and 40CdF 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye by the concrete grammar that 1: 50 mixing and doping of mass ratio prepares target are: press 40CdF 260BaF 21.6Er 2O 3Complex and 1: 50 ratio of orange-colored light absorbing dye mass ratio are got orange-colored light absorbing dye and 40CdF 260BaF 21.6Er 2O 3Put in orange-colored light absorbing dye and deionized water quality and put into deionized water than 1: 4 ratio, behind the ultrasonic dispersion 15min, be heated to boiling constant temperature 30min, filter and clean, put into crucible and heat up with the speed of 2 ℃/min, be heated to 500 ℃ and be incubated 3h, obtain 40CdF behind the cooling forming at muffle furnace 260BaF 21.6Er 2O 3Complex and orange-colored light absorbing dye are pressed the target of mass ratio mixing and doping preparation in 1: 50.
8. the preparation method who is used for the light-conversion nano-film of PDP demonstration as claimed in claim 6 is characterized in that, in second step, and 40CdF 260BaF 21.6Er 2O 3The concrete grammar of the preparation of complex is: with CdF 2, BaF 2, Er 2O 340: 60: 1.6 in molar ratio ratio mixes after grinding, and mix powder is put into sintering furnace is heated to 1000 ℃ of sintering 10min after annealing obtains complex 40CdF 260BaF 21.6Er 2O 3
9. as claim 6,7,8 arbitrary described preparation methods that are used for the light-conversion nano-film of PDP demonstration, it is characterized in that described orange-colored light absorbing dye is any one in tetra-tert tetraazatetradecane porphyrin cobalt, tetra-tert tetraazatetradecane porphyrin lead or the ethyl violet.
10. the light-conversion nano-film that the PDP of being used for as claimed in claim 1 shows is used to prepare light-filtering screened film.
CN2009100331200A 2009-06-12 2009-06-12 Light-conversion nano-film for PDP display, and preparation method thereof Expired - Fee Related CN101581808B (en)

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CN101899222A (en) * 2010-07-01 2010-12-01 北川天诺光电材料有限公司 Neon yellow light absorbing dye and application thereof
CN102753886A (en) * 2010-04-23 2012-10-24 海洋王照明科技股份有限公司 Light convergence device, manufacturing method thereof and solar battery system
CN102928074A (en) * 2012-10-24 2013-02-13 上海科润光电技术有限公司 Preparation of up-conversion luminescence imaging reinforced film
CN103235347A (en) * 2013-04-23 2013-08-07 上海洞舟实业有限公司 Method for preparing multi-band infrared laser detection device
CN109946924A (en) * 2019-02-21 2019-06-28 苏州星烁纳米科技有限公司 Resin combination and display device

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CN102753886A (en) * 2010-04-23 2012-10-24 海洋王照明科技股份有限公司 Light convergence device, manufacturing method thereof and solar battery system
CN102753886B (en) * 2010-04-23 2014-07-02 海洋王照明科技股份有限公司 Light convergence device, manufacturing method thereof and solar battery system
CN101899222A (en) * 2010-07-01 2010-12-01 北川天诺光电材料有限公司 Neon yellow light absorbing dye and application thereof
CN102928074A (en) * 2012-10-24 2013-02-13 上海科润光电技术有限公司 Preparation of up-conversion luminescence imaging reinforced film
CN103235347A (en) * 2013-04-23 2013-08-07 上海洞舟实业有限公司 Method for preparing multi-band infrared laser detection device
CN103235347B (en) * 2013-04-23 2016-07-13 上海洞舟实业有限公司 A kind of preparation of multiband detection of infrared laser device
CN109946924A (en) * 2019-02-21 2019-06-28 苏州星烁纳米科技有限公司 Resin combination and display device

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