CN110272662A - A kind of preparation method of large area light emitting film - Google Patents
A kind of preparation method of large area light emitting film Download PDFInfo
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- CN110272662A CN110272662A CN201910499401.9A CN201910499401A CN110272662A CN 110272662 A CN110272662 A CN 110272662A CN 201910499401 A CN201910499401 A CN 201910499401A CN 110272662 A CN110272662 A CN 110272662A
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- emitting film
- large area
- preparation
- light emitting
- area light
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
- C09K2211/1408—Carbocyclic compounds
- C09K2211/1425—Non-condensed systems
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
- C09K2211/1408—Carbocyclic compounds
- C09K2211/1433—Carbocyclic compounds bridged by heteroatoms, e.g. N, P, Si or B
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation methods of large area light emitting film, the following steps are included: step 1, by luminescent material and as the polyethylene glycol oxide of electrolyte, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium mixed dissolution is configured to ink in binary solvent；Step 2 strangles stick by wheat and ink is printed film forming, and made annealing treatment, and obtains the light-emitting film.The present invention introduces the excessive crystallization that dual solvent system inhibits electrolyte in printing ink, regulates and controls the secondary flow of ink than parameter by different Solute mass, and regulation print speed printing speed realizes the preparation of large area light emitting film.The light-emitting film excellent combination property being prepared in the present inventive method, be embodied in no strip flaw, mutually separate be uniformly distributed, carrier mobility height, it can be achieved that prepared by the high quality printing of high efficiency large area organic electro-optic device.
Description
Technical field
The present invention relates to a kind of preparation methods of large area light emitting film, belong to optoelectronic materials technology.
Background technique
Flexibility, large area, wearable display and luminaire will can become a part indispensable in life, be people
The life of class, production, existence are provided convenient and are ensured.Printed electronics and industrialized production have natural compatibility,
And the combination of the electronics and information industries such as illumination, display has become development trend.Wheat strangles stick printing technology and is generally difficult to overcome its print
The problems such as high roughness of brush film is with printing scratch is also easy to produce can not apply to always high quality printing preparation and shine and show
Device.
Summary of the invention
It is existing in the prior art to solve the object of the present invention is to provide a kind of preparation method of large area light emitting film
Generally use wheat strangle stick printing preparation Film roughness is big, uniformity is poor, and will appear material aggregation and needle pore defect
Problem.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of large area light emitting film, comprising the following steps:
Step 1, by luminescent material and as the polyethylene glycol oxide of electrolyte, three propylene of ethoxylated trimethylolpropane
Acid esters, trifluoromethanesulfonic acid lithium mixed dissolution are configured to ink in binary solvent；
Step 2 strangles stick by wheat and ink is printed film forming, and made annealing treatment, and obtains the light-emitting film.
Preferably, in the step 1, the concentration of luminescent material is 3~7mg mL-1；Luminescent material, polyethylene glycol oxide, second
Oxygroup trimethylolpropane trimethacrylate, trifluoromethanesulfonic acid lithium mass ratio be 10:2:10:2.
Preferably, the luminescent material be it is poly- [2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene, it is poly- [2,
5- bis- (3 ', 7 '-dimethyl-octa oxygroup) -1,4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4-
One of phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }].
Preferably, in the step 1, binary solvent is cyclohexanone and tetrahydrofuran, toluene and tetrahydrofuran, cyclohexanone
With methylene chloride or one of toluene and methylene chloride.
Preferably, in the binary solvent, two kinds of solvent volume ratio 3:1~1:3.
Preferably, in the step 2, the temperature of annealing is 80~120 DEG C.
Preferably, in the step 2, wheat strangles stick print speed printing speed in 5~30m s-1In range.
Preferably, the light-emitting film is with a thickness of 60~1000nm.
The utility model has the advantages that the present invention introduces the excessive crystallization that dual solvent system inhibits electrolyte in printing ink, pass through
Different Solute mass carries out large area light emitting under conditions of print speed printing speed is variable than the secondary flow of parameter regulation ink
The printing of film.The light-emitting film excellent combination property being prepared in the present inventive method, be embodied in no strip flaw,
Mutually being uniformly distributed of separation, carrier mobility is high, it can be achieved that high efficiency large area organic electro-optic device high quality printing system
It is standby.
Detailed description of the invention
Fig. 1 is the optical microscopy characterization of light-emitting film prepared by the embodiment of the present invention；
Fig. 2 is the atomic force microscope characterization of light-emitting film prepared by the embodiment of the present invention；
Fig. 3 is the light of light-emitting film (rear) prepared by light-emitting film prepared by the prior art (preceding) and present example
Learn microscopic characterization.
Specific embodiment
The specific embodiment of the application is described in further detail below.Following embodiment will be helpful to this field
Technical staff further understand the application, but do not limit the application in any form.It should be pointed out that the general of this field
For logical technical staff, without departing from the concept of this application, several changes and improvements can also be made, these are belonged to
The protection scope of the application.
Embodiment 1
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
For solution in the binary solvent that cyclohexanone and tetrahydrofuran volume ratio are 3:1, solution concentration is 10mg mL-1.Then, match above-mentioned
The 0.2mL polyethylene oxide solutions of system, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid
Lithium solution is added to the poly- [in 2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene luminescent material, on 0.6mL of 10mg
The binary solvent stated further dissolves, and is stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 500nm.
Embodiment 2
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
For solution in the binary solvent that toluene and tetrahydrofuran volume ratio are 3:1, solution concentration is 10mg mL-1.Then, by above-mentioned preparation
0.2mL polyethylene oxide solutions, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid lithium
Solution is added to the poly- [above-mentioned with 0.6mL in 2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene luminescent material of 10mg
Binary solvent further dissolve, be stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 1000nm.
Embodiment 3
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
Solution is in cyclohexanone and methylene chloride volume than in the binary solvent for 3:1, solution concentration is 10mg mL-1.Then, match above-mentioned
The 0.2mL polyethylene oxide solutions of system, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid
Lithium solution is added to the poly- [in 2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene luminescent material, on 0.6mL of 10mg
The binary solvent stated further dissolves, and is stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 60nm.
Embodiment 4
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
Solution is in toluene and methylene chloride volume than in the binary solvent for 3:1, solution concentration is 10mg mL-1.Then, by above-mentioned preparation
0.2mL polyethylene oxide solutions, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid lithium
Solution is added to the poly- [above-mentioned with 0.6mL in 2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene luminescent material of 10mg
Binary solvent further dissolve, be stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 300nm.
Embodiment 5
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
For solution in the binary solvent that cyclohexanone and tetrahydrofuran volume ratio are 3:1, solution concentration is 10mg mL-1.Then, match above-mentioned
The 0.2mL polyethylene oxide solutions of system, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid
Lithium solution is added to poly- [{ 2,5- bis- (3 ', 7 '-dimethyl-octa oxygroup) -1,4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-of 10mg
Dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- benzene second
Alkynes }] in luminescent material, is further dissolved with 0.6mL above-mentioned binary solvent, be stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 400nm.
Embodiment 6
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
For solution in the binary solvent that toluene and tetrahydrofuran volume ratio are 3:1, solution concentration is 10mg mL-1.Then, by above-mentioned preparation
0.2mL polyethylene oxide solutions, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid lithium
Solution is added to poly- [{ 2,5- bis- (3 ', 7 '-dimethyl-octa oxygroup) -1,4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-two of 10mg
Methyl octyloxy) phenyl) -1,4- phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }]
It in luminescent material, is further dissolved with 0.6mL above-mentioned binary solvent, is stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 800nm.
Embodiment 7
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
Solution is in cyclohexanone and methylene chloride volume than in the binary solvent for 3:1, solution concentration is 10mg mL-1.Then, match above-mentioned
The 0.2mL polyethylene oxide solutions of system, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid
Lithium solution is added to poly- [{ 2,5- bis- (3 ', 7 '-dimethyl-octa oxygroup) -1,4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-of 10mg
Dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- benzene second
Alkynes }] in luminescent material, is further dissolved with 0.6mL above-mentioned binary solvent, be stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 100nm.
Embodiment 8
Step 1: polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate, trifluoromethanesulfonic acid lithium difference is molten
Solution is in toluene and methylene chloride volume than in the binary solvent for 3:1, solution concentration is 10mg mL-1.Then, by above-mentioned preparation
0.2mL polyethylene oxide solutions, 1mL ethoxylated trimethylolpropane triacrylate solution, 0.2mL trifluoromethanesulfonic acid lithium
Solution is added to poly- [{ 2,5- bis- (3 ', 7 '-dimethyl-octa oxygroup) -1,4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-two of 10mg
Methyl octyloxy) phenyl) -1,4- phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }]
It in luminescent material, is further dissolved with 0.6mL above-mentioned binary solvent, is stirred overnight to form printing ink at 80 DEG C.
Step 2: wheat is strangled rod speed control in 20m s-1, the ink in the first step is printed as film, which is put
It sets and anneals 30 minutes on 100 DEG C of warm table.
Light-emitting film obtained is with a thickness of 600nm.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation method of large area light emitting film, it is characterised in that: the following steps are included:
Step 1, by luminescent material with as the polyethylene glycol oxide of electrolyte, ethoxylated trimethylolpropane triacrylate,
Trifluoromethanesulfonic acid lithium mixed dissolution is configured to ink in binary solvent；
Step 2 strangles stick by wheat and ink is printed film forming, and made annealing treatment, and obtains the light-emitting film.
2. the preparation method of large area light emitting film according to claim 1, it is characterised in that: in the step 1, hair
The concentration of luminescent material is 3~7mg mL-1；Luminescent material, polyethylene glycol oxide, ethoxylated trimethylolpropane triacrylate,
The mass ratio of trifluoromethanesulfonic acid lithium is 10:2:10:2.
3. the preparation method of large area light emitting film according to claim 1 or 2, it is characterised in that: the luminescent material
Be it is poly- [2- methoxyl group -5- (2 '-ethyls-ethyoxyl)-Isosorbide-5-Nitrae-styrene, it is poly- [2,5- bis- (3 ', 7 '-dimethyl-octa oxygroups) -1,
4- phenylacetylene }-co- { 3- (4 '-(3 ", 7 "-dimethyl-octa oxygroup) phenyl) -1,4- phenylacetylene }-co- { 3- (3 '-(3 ", 7 "-two
One of methyl octyloxy) phenyl) -1,4- phenylacetylene }].
4. the preparation method of large area light emitting film according to claim 1, it is characterised in that: in the step 1, two
First solvent is in cyclohexanone and tetrahydrofuran, toluene and tetrahydrofuran, cyclohexanone and methylene chloride or toluene and methylene chloride
It is a kind of.
5. the preparation method of large area light emitting film according to claim 4, it is characterised in that: in the binary solvent,
Two kinds of solvent volume ratio 3:1~1:3.
6. the preparation method of large area light emitting film according to claim 1, it is characterised in that: in the step 2, move back
The temperature of fire processing is 80~120 DEG C.
7. the preparation method of large area light emitting film according to claim 1, it is characterised in that: in the step 2, wheat
Stick print speed printing speed is strangled in 5~30m s-1In range.
8. the preparation method of large area light emitting film according to claim 1, it is characterised in that: the light-emitting film thickness
For 60~1000nm.
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| CN201910499401.9A CN110272662A (en) | 2019-06-11 | 2019-06-11 | A kind of preparation method of large area light emitting film |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102782083A (en) * | 2009-09-10 | 2012-11-14 | 住友化学株式会社 | Ionic salt combinations in polymer electroluminescent inks |
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2019
- 2019-06-11 CN CN201910499401.9A patent/CN110272662A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102782083A (en) * | 2009-09-10 | 2012-11-14 | 住友化学株式会社 | Ionic salt combinations in polymer electroluminescent inks |
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