CN102201548B - Substrate for flexible luminescent device and preparation method thereof - Google Patents
Substrate for flexible luminescent device and preparation method thereof Download PDFInfo
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- CN102201548B CN102201548B CN201110096378.2A CN201110096378A CN102201548B CN 102201548 B CN102201548 B CN 102201548B CN 201110096378 A CN201110096378 A CN 201110096378A CN 102201548 B CN102201548 B CN 102201548B
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Abstract
The invention discloses a substrate for a flexible luminescent device, which comprises a flexible substrate and a conductive layer which are formed in one of the following two modes: 1, the flexible substrate is made of a transparent dielectric polymer material, the conductive layer is a thin-layer carbon nanotube, and inorganic luminous nanoparticles are filled in a gap of the thin-layer carbon nanotube; and 2, the flexible substrate is made of a transparent dielectric polymer material doped with the inorganic luminous nanoparticles, the conductive layer is made of the thin-layer carbon nanotube, and the transparent dielectric polymer material doped with the inorganic luminous nanoparticles is filled in the gap of the thin-layer carbon nanotube. By the substrate, the problems of low surface smoothness of the thin-layer carbon nanotube and low bonding force between the carbon nanotube and the flexible substrate are solved, and the electrical conductivity of the conductive layer and the blocking ability of the substrate on water oxygen are improved.
Description
Technical field
The present invention relates to organic optoelectronic technical field, be specifically related to a kind of substrate used in luminescent device and preparation method thereof.
Background technology
Photoelectron technology is the very high industry of scientific and technological content developing rapidly after microelectric technique.Along with the fast development of photoelectron technology, the O-E Products such as solar cell, optical image transducer, flat-panel screens, thin-film transistor are all full-fledged gradually, and they have improved people's life greatly.Meanwhile, opto-electronic information technology, in the extensive use of social life every field, has also been created growing great market.Developed country is all using optoelectronic information industry as one of field of giving priority to, and the competition of the field of opto-electronic information just launches at world wide.
Photoelectron technology is the very high industry of scientific and technological content developing rapidly after microelectric technique.Along with the fast development of photoelectron technology, the O-E Products such as solar cell, optical image transducer, flat-panel screens, thin-film transistor are all full-fledged gradually, and they have improved people's life greatly.Meanwhile, opto-electronic information technology, in the extensive use of social life every field, has also been created growing great market.Developed country is all using optoelectronic information industry as one of field of giving priority to, and the competition of the field of opto-electronic information just launches at world wide.
Organic optoelectronic device is mostly that preparation is at rigid substrates (on glass or silicon chip), although they have good device performance, anti-vibration at present, shock proof ability a little less than, weight is relatively heavier, and it is very not convenient to carry, and in the application of some occasion, is very restricted.People start to attempt organic optoelectronic device is deposited on flexible base, board rather than on rigid substrates.
With flexible base, board, replacing the benefit of rigid substrates is that lighter, the difficult fragmentation of product, institute take up space little and be more convenient for carrying.But, although there are these advantages, with flexible base, board, replace rigid substrates also to have many restrictions, the preparation of flexible device still has many underlying issues to need to solve.For flexible substrate, because the profile pattern of flexible substrate is also far away from rigid substrate, and flexible substrate is carried out to surface smoothing, to process equipment and the technology difficulty of wanting special larger, improved the production cost of substrate; The water of flexible substrate, oxygen permeability be much larger than rigid substrate, causes opto-electronic device to be subject to the impact of the water oxygen that sees through from substrate, reduced the performance of device.
For electrode layer, conventional electrode layer material In
2o
3: SnO
2(ITO) there is following shortcoming in the electrode as flexible base, board: the indium in (1) ITO has severe toxicity, harmful in preparation and application; (2) In in ITO
2o
3expensive, cost is higher; (3) ito thin film is vulnerable to the reduction of hydrogen plasma, and effect reduces, and this phenomenon also can occur under low temperature, low plasma density; (4) can there is because of the bending of flexible substrate the phenomenon that conductivity declines in the ito thin film in flexible substrate; (5) adopt thick ITO layer can reduce light transmittance, the light of 50-80% sponges at glass, ITO and organic layer, adopts thin ITO layer process difficulty larger.Because having high mechanical strength and elasticity and good conductor characteristics, carbon nano-tube receives publicity.2006, the people such as Canadian R.Martel (Appl.Phys.lett., 2006,88,183104) pointed out that the increase of carbon nano-tube film thickness can reduce visible light transmissivity and the resistance of film.For carbon nano-tube film is obtained compared with high visible light transmissivity, just must reduce the thickness of carbon nano-tube film, increased so again the sheet resistance of carbon nano-tube film, make the sheet resistance of carbon nano-tube film obtain 10
3Ω/sq magnitude, has reduced carbon nano-tube film conductivity.
Therefore,, if can solve above-mentioned these problems, will make opto-electronic device obtain applying more widely and development more fast.
Summary of the invention
Technical problem to be solved by this invention is how a kind of substrate used in luminescent device and preparation method thereof is provided, this substrate has solved the poor problem of adhesion between thin layer carbon nano tube surface poor flatness and carbon nano-tube and flexible substrate, has improved conductivity and the obstructing capacity of substrate to water oxygen of conductive layer.
Technical problem proposed by the invention is to solve like this: a kind of substrate used in luminescent device is provided, comprise flexible substrate and conductive layer, it is characterized in that, a kind of in following two kinds of modes forms for described flexible substrate and conductive layer: 1. flexible substrate is transparent dielectricity polymeric material, conductive layer is thin layer carbon nano-tube, is filled with inorganic light-emitting nano particle in the space of described thin layer carbon nano-tube; 2. flexible substrate is the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, conductive layer is thin layer carbon nano-tube, the transparent dielectricity polymeric material that is filled with doping inorganic light-emitting nano particle in the space of described thin layer carbon nano-tube, the thickness of described thin layer carbon nano-tube is less than or equal to 100nm.
According to substrate used in luminescent device provided by the present invention, it is characterized in that, described inorganic light-emitting nanoparticle size is 1～50nm, 2. in kind mode the doping mass ratio of inorganic light-emitting nano particle be less than or equal to 40%.
According to substrate used in luminescent device provided by the present invention, it is characterized in that, described inorganic light-emitting nano particle is that to take sulfide, oxide, fluoride, phosphate, vanadate, niobates, aluminate, molybdate etc. be luminous host, usings the light-emitting particles of rare earth lanthanide as activator and co-activator.
According to substrate used in luminescent device provided by the present invention, it is characterized in that, described sulfide comprises zinc sulphide, lanthanum sulfide, calcium sulfide, cerium sulphide, praseodymium sulfide, neodymium sulfide, samaric sulfide and gadolinium sulfide; Described oxide comprises zinc oxide, yittrium oxide, titanium oxide, gadolinium oxide and luteium oxide; Described fluoride comprises yttrium fluoride, gadolinium fluoride, lanthanum fluoride and cerium fluoride; Described phosphate comprises lanthanum orthophosphate, Gadolinium monophosphate, strontium phosphate, yttrium phosphate and barium phosphate; Described vanadate comprises gadolinium vanadate, Yttrium Orthovanadate, vanadic acid lanthanum, cerium vanadate, vanadic acid calcium, lead vanadate and vanadic acid strontium; Described niobates comprises calcium niobate, niobic acid yttrium, niobic acid gadolinium and niobic acid lutetium; Described aluminate comprises yttrium aluminate, barium aluminate, aluminic acid gadolinium, calcium aluminate and strontium aluminate; Described molybdate comprises lanthanum molybdate, strontium molybdate and barium molybdate; Described rare earth lanthanide comprises europium, samarium, erbium, neodymium, terbium, dysprosium, samarium, cerium, ytterbium and praseodymium.
According to substrate used in luminescent device provided by the present invention, it is characterized in that, described transparent dielectricity polymeric material is one or more in polyethylene, polymethyl methacrylate, Merlon, polyurethanes, polyimides, vinyl chloride-vinyl acetate resin, polyacrylic acid, PAEK, Kynoar, polyester, PEN, polyacrylate, poly-paraphenylene terephthalamide's trimethyl hexamethylene diamine, polybutene and polyvinyl alcohol.
A preparation method for substrate used in luminescent device, is characterized in that, comprises the following steps:
1. the rigid substrates (as glass or silicon chip) that effects on surface roughness is less than 1nm cleans, and after cleaning, with drying nitrogen, dries up;
2. take the mode of spin coating or spraying or self assembly or inkjet printing or silk screen printing to prepare carbon nanotube layer on clean rigid substrates;
3. the transparent dielectricity polymeric layer of spin coating or spraying doping inorganic light-emitting nano particle on carbon nanotube layer, first spin coating or drip to be coated with or spraying containing the solution of inorganic light-emitting nano particle, spin coating or drip to be coated with or to spray transparent dielectricity polymeric layer again, described transparent dielectricity polymeric material is polyethylene, polymethyl methacrylate, Merlon, polyurethanes, polyimides, vinyl chloride-vinyl acetate resin, polyacrylic acid, PAEK, Kynoar, polyester, PEN, polyacrylate, poly-paraphenylene terephthalamide's trimethyl hexamethylene diamine, one or more in polybutene and polyvinyl alcohol,
4. the substrate of the good transparent dielectricity polymeric material of spin coating is toasted;
5. the transparent dielectricity polymeric layer of the transparent dielectricity polymeric layer by carbon nanotube layer and after solidifying or doping inorganic light-emitting nano particle is peeled off rigid substrates surface, forms compliant conductive substrate;
6. test the parameters of transmitance, conductivity and the surface topography of compliant conductive substrate.
Beneficial effect of the present invention: have inorganic light-emitting nano particle in conductive layer of the present invention, make conductive layer luminous under exciting light irradiates, not only strengthen the luminous intensity of the luminescent device based on this substrate, and simplified the structure of the luminescent device based on this substrate and required material; Conductive layer of the present invention is prepared on the little rigid substrates of roughness, in conductive layer space, be filled with the transparent dielectricity polymeric material of inorganic light-emitting nano particle or doping inorganic light-emitting nano particle, utilize adhesion between transparent dielectricity polymeric material and electrode material to be better than the characteristic of electrode material and rigid substrates, electrode layer by preparation on the little rigid substrates of roughness is peeled off, and has improved the evenness of the electrode layer surface in flexible substrate; Adopt transparent dielectricity polymeric material as effective the seeing through of block water oxygen of flexible substrate, transparent dielectricity polymeric material of the present invention has the feature of high visible light transmissivity simultaneously, and substrate visible light transmissivity is improved.
Accompanying drawing explanation
Fig. 1 is the structural representation of the substrate used in luminescent device of embodiment of the present invention 1-9;
Fig. 2 is the visible light transmissivity of the substrate in the embodiment of the present invention 1.
Wherein, 1, flexible substrate, 2, conductive layer.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the invention will be further described:
Technical scheme of the present invention is to provide a kind of substrate used in luminescent device, and as shown in Figure 1, the structure of device comprises flexible substrate 1, conductive layer 2.
The support that in the present invention, flexible substrate 1 is conductive layer, it has good bending performance, the ability that has certain anti-steam and oxygen infiltration, there are good chemical stability and thermal stability, conductive layer 2 requires to have good conductive capability, flexible substrate 1 and conductive layer 2 consist of following two kinds of modes: 1. flexible substrate is transparent dielectricity polymeric material, and conductive layer is thin layer carbon nano-tube, is filled with inorganic light-emitting nano particle in the space of described thin layer carbon nano-tube; 2. flexible substrate is the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, and conductive layer is thin layer carbon nano-tube, is filled with the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle in the space of described thin layer carbon nano-tube.
Below specific embodiments of the invention:
Board structure as shown in Figure 1, flexible substrate 1 adopts transparent dielectricity polymeric material, described transparent dielectricity polymeric material is polyethylene, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 50nm, and described carbon nano-tube layer thickness is 100 nanometers.
Preparation method is as follows:
1. the silicon substrate that effects on surface roughness is less than 1nm cleans, and after cleaning, with drying nitrogen, dries up;
2. even carbon nanotube is dispersed in solvent, takes spin coating mode to prepare carbon nanotube layer on clean silicon substrate, during spin coating, rotating speed is 4000 revolutions per seconds, duration 50 seconds, and thickness is about 100 nanometers;
3. on carbon nanotube layer, spray the solution of inorganic light-emitting nano particle, silicon substrate placed 30 minutes in the environment of 80 ℃, remove solvent remaining in carbon nanotube layer, then on carbon nanotube layer spraying polyethylene solution;
4. the substrate of the good polyethylene film of spin coating is toasted;
5. carbon nanotube layer and polyethylene film are peeled off to silicon substrate surface, form compliant conductive substrate;
6. test the parameters of transmitance, conductivity and the surface topography of compliant conductive substrate.
Board structure as shown in Figure 1, flexible substrate 1 adopts transparent dielectricity polymeric material polymethyl methacrylate, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 30nm, and described carbon nano-tube layer thickness is 90 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 3
Board structure as shown in Figure 1, flexible substrate 1 adopts transparent dielectricity polymeric material, described transparent dielectricity polymeric material comprises 90% polymethyl methacrylate, 10% Merlon, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 25nm, and described carbon nano-tube layer thickness is 80 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 4
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 5%, described transparent dielectricity polymeric material comprises 90% polymethyl methacrylate, 10% Merlon, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 15nm, and described carbon nano-tube layer thickness is 70 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 5
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 10%, described transparent dielectricity polymeric material comprises 80% polyurethanes, 10% polyimides and 10% polybutene, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 10nm, and described carbon nano-tube layer thickness is 60 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 6
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 15%, described transparent dielectricity polymeric material comprises 85% Kynoar, 10% polyethylene and 5% polybutene, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 10nm, and described carbon nano-tube layer thickness is 50 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 7
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 20%, described transparent dielectricity polymeric material comprises 88% polyester, 6% polyethylene, 4% polybutene and 2% Kynoar, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 1nm, and described carbon nano-tube layer thickness is 40 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 8
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 30%, described transparent dielectricity polymeric material comprises 80% polyester, 10% polymethyl methacrylate, 6% PEN and 4% Kynoar, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 5nm, described carbon nano-tube layer thickness is 70 nanometers.
Preparation method is similar to embodiment 1.
Embodiment 9
Board structure as shown in Figure 1, flexible substrate 1 adopts the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the doping mass ratio of described inorganic light-emitting nano particle is 40%, described transparent dielectricity polymeric material comprises 81% polyimides, 9% PEN, 5% polyurethanes and 5% polyacrylate, conductive layer 2 adopts carbon nano-tube, in the space of described carbon nanotube layer, fill the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, described inorganic light-emitting nano particle is of a size of 15nm, described carbon nano-tube layer thickness is 80 nanometers.
Preparation method is similar to embodiment 1.
Claims (4)
1. the preparation method of a substrate used in luminescent device, this substrate comprises flexible substrate and conductive layer, a kind of in following two kinds of modes forms for described flexible substrate and conductive layer: 1. flexible substrate is transparent dielectricity polymeric material, conductive layer is thin layer carbon nano-tube, is filled with inorganic light-emitting nano particle in the space of described thin layer carbon nano-tube; 2. flexible substrate is the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, conductive layer is thin layer carbon nano-tube, in the space of described thin layer carbon nano-tube, be filled with the transparent dielectricity polymeric material of doping inorganic light-emitting nano particle, the thickness of described thin layer carbon nano-tube is less than or equal to 100nm, it is characterized in that, comprise the following steps:
1. the rigid substrates that effects on surface roughness is less than 1nm cleans, and after cleaning, with drying nitrogen, dries up;
2. take the mode of spin coating or spraying or self assembly or inkjet printing or silk screen printing to prepare carbon nanotube layer on clean rigid substrates;
3. the transparent dielectricity polymeric layer of spin coating or spraying doping inorganic light-emitting nano particle on carbon nanotube layer, first spin coating or drip to be coated with or spraying containing the solution of inorganic light-emitting nano particle, spin coating or drip to be coated with or to spray transparent dielectricity polymeric layer again, described transparent dielectricity polymeric material is polyethylene, polymethyl methacrylate, Merlon, polyurethanes, polyimides, vinyl chloride-vinyl acetate resin, polyacrylic acid, PAEK, Kynoar, polyester, PEN, polyacrylate, poly-paraphenylene terephthalamide's trimethyl hexamethylene diamine, one or more in polybutene and polyvinyl alcohol,
4. the substrate of the good transparent dielectricity polymeric material of spin coating is toasted;
5. the transparent dielectricity polymeric layer of carbon nanotube layer and transparent dielectricity polymeric layer or doping inorganic light-emitting nano particle is peeled off to rigid substrates surface, form compliant conductive substrate;
6. test the parameter of transmitance, conductivity and the surface topography of compliant conductive substrate.
2. the preparation method of substrate used in luminescent device according to claim 1, is characterized in that, described inorganic light-emitting nanoparticle size is 1～50nm, 2. in kind mode the doping mass ratio of inorganic light-emitting nano particle be less than or equal to 40%.
3. the preparation method of substrate used in luminescent device according to claim 1, it is characterized in that, described inorganic light-emitting nano particle is to take sulfide, oxide, fluoride, phosphate, vanadate, niobates, aluminate or molybdate as luminous host, usings the light-emitting particles of rare earth lanthanide as activator and co-activator.
4. the preparation method of substrate used in luminescent device according to claim 3, is characterized in that, described sulfide comprises zinc sulphide, lanthanum sulfide, calcium sulfide, cerium sulphide, praseodymium sulfide, neodymium sulfide, samaric sulfide or gadolinium sulfide; Described oxide comprises zinc oxide, yittrium oxide, titanium oxide, gadolinium oxide or luteium oxide; Described fluoride comprises yttrium fluoride, gadolinium fluoride, lanthanum fluoride or cerium fluoride; Described phosphate comprises lanthanum orthophosphate, Gadolinium monophosphate, strontium phosphate, yttrium phosphate or barium phosphate; Described vanadate comprises gadolinium vanadate, Yttrium Orthovanadate, vanadic acid lanthanum, cerium vanadate, vanadic acid calcium, lead vanadate or vanadic acid strontium; Described niobates comprises calcium niobate, niobic acid yttrium, niobic acid gadolinium or niobic acid lutetium; Described aluminate comprises yttrium aluminate, barium aluminate, aluminic acid gadolinium, calcium aluminate or strontium aluminate; Described molybdate comprises lanthanum molybdate, strontium molybdate or barium molybdate; Described rare earth lanthanide comprises europium, samarium, erbium, neodymium, terbium, dysprosium, samarium, cerium, ytterbium or praseodymium.
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| CN103963408A (en) * | 2014-04-30 | 2014-08-06 | 电子科技大学 | Method for preparing high dielectric polymer composite film |
| CN104616838B (en) * | 2015-02-10 | 2018-02-06 | 京东方科技集团股份有限公司 | The preparation method and electronic device of a kind of electronic device |
| CN104766932A (en) * | 2015-04-22 | 2015-07-08 | 电子科技大学 | Biodegradable baseplate used for soft light electron device and manufacturing method thereof |
| US20180331312A1 (en) * | 2015-11-04 | 2018-11-15 | Guangzhou Chinaray Optoelectronic Materials Ltd. | Electroluminescent device, preparation method thereof, and ink formulation |
| CN113447174A (en) * | 2021-06-25 | 2021-09-28 | 安徽熙泰智能科技有限公司 | Micro OLED laminated packaging structure stress testing method and Micro OLED laminated packaging structure |
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