CN106947321A - A kind of ink, preparation method and application for being used to make cushion - Google Patents
A kind of ink, preparation method and application for being used to make cushion Download PDFInfo
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- CN106947321A CN106947321A CN201710258766.3A CN201710258766A CN106947321A CN 106947321 A CN106947321 A CN 106947321A CN 201710258766 A CN201710258766 A CN 201710258766A CN 106947321 A CN106947321 A CN 106947321A
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- 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
- C09D11/30—Inkjet printing inks
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- C—CHEMISTRY; METALLURGY
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- 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
- C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- 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
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/135—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising mobile ions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
- H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
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- Inks, Pencil-Leads, Or Crayons (AREA)
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Abstract
This disclosure relates to which a kind of cushion for being used to make ink of flexible organic light emission electrochemical cell cushion and preparation method and application and be prepared with this ink, the ink for making flexible organic light emission electrochemical cell cushion includes：Poly- (vinyl cinnamate), poly- (9,9 dioctyl fluorene), polymeric additive and organic solvent；Wherein, the concentration of poly- (vinyl cinnamate) is 5 40mg/mL in the ink, and the concentration of poly- (9,9 dioctyl fluorene) is 0.5 5mg/mL, and the weight ratio that the polymeric additive accounts for the ink is 1 10 weight %.The ink of the disclosure can be used for printing one layer of cushion between luminescent layer and negative electrode, and cushion can not only obstruct the infiltration of silver inks water but also can transmit electronics, so as to realize the inkjet printable of negative electrode, realize that free patterning is luminous in the case of without mask plate.
Description
Technical field
This disclosure relates to organic light emission electrochemical cell art field, in particular it relates to which a kind of be used to make flexible organic
Ink of light-emitting electrochemical cell cushion and preparation method and application and the cushion prepared with this ink.
Background technology
In recent years, preparing organic light emitting film device for whole soln method has had more extensive research, it with tradition
Evaporation coating method compare, have the advantages that quick, energy-conservation, stock utilization are high.Current solwution method is prepared in device research mostly
That single or multiple lift is prepared using solwution method, and can not realize whole soln prepare, whole soln prepare in it is the most key the problem of it
One is the problem of being mutually dissolved infiltration between each layer solution, generally require above and below two interlayers use orthogonal solvents, with electrode ink
The cushion of water contact should be able to also self-crosslinking, from without influenceing each layer to be played a part of, What is more can improve each
The performance of layer.
Traditional Organic Light Emitting Diode (OLED) device mainly includes machine small molecule light emitting diode and polymer hair
Optical diode.Compared with light emitting diode, organic light emission electrochemical cell (Organic Light-Emitting
Electrochemical Cells, OLEC) luminescence mechanism difference, some unique advantages are made it have, such as relatively low operation electricity
Pressure, higher electronics/photon conversion efficiency and higher power efficiency etc..More importantly it is, organic light emission electrochemical cell
Need not compared with low work function material as negative electrode, the electrode material of these low work functions is often unstable in atmosphere.Meanwhile,
Luminescent layer in organic light emission electrochemical cell in situ can produce p-n junction, be conducive to electronics and hole luminous from the two poles of the earth injection.Cause
This, compared to Organic Light Emitting Diode, organic light emission electrochemical cell is relatively low to the roughness requirements of electrode material surface, is conducive to
Large-scale production.
The preparation technology of organic light emission electrochemical cell (OLEC) is relatively easy, and luminescent layer typically uses spin coating proceeding system
It is standby, and electrode is still prepared using vacuum evaporation process, the silver inks water of current commercialization is mainly the ink of water system or alcohol system, meeting
Luminescent layer in organic light emission electrochemical cell is caused to dissolve or permeated, so as to cause element leakage, especially for transition
The device as luminescent layer of metal complex.
The content of the invention
The purpose of the disclosure is：First aspect provides a kind of for making flexible organic light emission electrochemical cell cushion
Ink, second aspect provides a kind of preparation method for being used to make the ink of flexible organic light emission electrochemical cell cushion, the
Three aspects provide the flexible organic light emission electrochemical cell cushion of ink making that a kind of use disclosure first aspect is provided
Method, fourth aspect provides a kind of flexible organic light emission electrochemical cell of making provided by the disclosure third aspect and delays
The flexible organic light emission electrochemical cell cushion made by the method for layer is rushed, the disclosure passes through for making flexible organic light emission
The ink of electrochemical cell cushion can realize the printing of cushion.
To achieve these goals, disclosure first aspect is used to make flexible organic light emission electrochemistry there is provided one kind
The ink of battery buffer layer, including：Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes), polymeric additive and organic molten
Agent；Wherein, the concentration of poly- (vinyl cinnamate) is 5-40mg/mL in the ink, and the concentration of poly- (9,9- dioctyl fluorene) is
0.5-5mg/mL, the weight ratio that the polymeric additive accounts for the ink is 1-10 weight %, the polymeric additive
Weight average molecular weight is 10000-50000.
Optionally, the organic solvent is at least one in toluene, methyl phenyl ethers anisole, DMF or chlorobenzene
Kind, the polymeric additive is polystyrene and/or polymethyl methacrylate.
Optionally, the organic solvent is toluene and/or methyl phenyl ethers anisole.
Optionally, poly- (vinyl cinnamate) and the weight ratio of poly- (9,9- dioctyl fluorene) are (5-20)：1.
There is provided a kind of ink for being used to make flexible organic light emission electrochemical cell cushion for disclosure second aspect
Preparation method, including：Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes) and polymeric additive and organic solvent is mixed
Close, obtain ink；Wherein, the concentration of poly- (vinyl cinnamate) is 5-40mg/mL, poly- (9,9- dioctyl fluorene) in the ink
Concentration be 0.5-5mg/mL, the polymeric additive account for the ink weight ratio be 1-10 weight %, the polymer
The weight average molecular weight of additive is 10000-50000.
Optionally, the organic solvent is at least one in toluene, methyl phenyl ethers anisole, DMF or chlorobenzene
Kind, the polymeric additive is polystyrene and/or polymethyl methacrylate.
Optionally, the organic solvent is toluene and/or methyl phenyl ethers anisole.
Optionally, poly- (vinyl cinnamate) and the weight ratio of poly- (9,9- dioctyl fluorene) are (5-20)：1.
Optionally, methods described also includes：By the addition of poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes) and polymer
Agent is stirred successively after being mixed with organic solvent, ultrasonic and filtering.
Optionally, the time of the stirring is 0.5-1 hours, and the ultrasonic time is 1-10min, and supersonic frequency is
20-40kHz, the precision of the filtering is 0.1-0.5 microns.
The disclosure third aspect makes flexible organic hair there is provided the ink that a kind of use disclosure first aspect is provided
The method of photoelectrochemical cell cushion, including：Make ink film；Wherein, it is described make ink film mode be selected from
At least one in inkjet printing, silk-screen printing, spin coating and blade coating；Gained ink film, which is placed under ultraviolet light, makes its internal hair
Raw cross-linking reaction.
Optionally, the mode for making ink film is inkjet printing and/or silk-screen printing.
There is provided a kind of flexible organic light emission electricity of making provided by the disclosure third aspect for disclosure fourth aspect
Flexible organic light emission electrochemical cell cushion made by the method for chemical cell cushion.
There is provided for making flexible organic light emission electrochemical cell cushion by allocating the composition of ink for the disclosure
Ink, can not only obstruct the infiltration of silver inks water but also can transmit the buffering of electronics by printing one layer between luminescent layer and negative electrode
Layer, so as to realize the inkjet printable of negative electrode, realizes that free patterning is luminous in the case of without mask plate.
In addition, the cushion that the disclosure is provided has electron transport property, solvent used will not destroy transition metal and match somebody with somebody
The luminescent layer of compound class, the film itself that ink-jet is formed can be crosslinked, and the ink sprayed afterwards will not permeate, and be heated even if upper strata
Cushion will not be dissolved.
Other feature and advantage of the disclosure will be described in detail in subsequent embodiment part.
Embodiment
Embodiment of this disclosure is described in detail below.It should be appreciated that described herein specific
Embodiment is merely to illustrate and explained the disclosure, is not limited to the disclosure.
Prior art prepares active layer (luminescent layer) film on tin indium oxide (ITO) electrode, then be deposited with silver electrode or
Aluminium electrode.Top electrode is mainly the method using vacuum evaporation, and apparatus expensive, preparation time is very long, and most of needs are in hand
Operated in casing.Other electrode evaporation is, it is necessary to which the mask plate of various patterns, the mask plate price of patterns of high precision is very high
It is expensive.Cushion refers in thin film electronic device that layer or several layers of of active layer (luminescent layer) between electrode can be divided into anode
Cushion and cathode buffer layer, main function are transmission electronics or hole.
Disclosure first aspect is used to make the ink of flexible organic light emission electrochemical cell cushion there is provided a kind of,
Including：Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes), polymeric additive and organic solvent；Wherein, in the ink
The concentration of poly- (vinyl cinnamate) is 5-40mg/mL, and the concentration of poly- (9,9- dioctyl fluorene) is 0.5-5mg/mL, the polymerization
The weight ratio that thing additive accounts for the ink is 1-10 weight %；Preferably, in the ink poly- (vinyl cinnamate) it is dense
Spend for 10-20mg/mL, the concentration of poly- (9,9- dioctyl fluorene) is 1-3mg/mL, and the polymeric additive accounts for the ink
Weight ratio is 3-6 weight %, and the weight average molecular weight of the polymeric additive is 10000-50000.
According to the disclosure in a first aspect, in order to realize organic light emission electrochemical cell (OLEC) device whole soln prepare,
Prepared by even full inkjet printing, the disclosure is directed to organic light emission electrochemical cell of the transient metal complex as luminescent layer,
A kind of organic buffer layer ink orthogonal with luminescent layer is prepared for by many experiments, mainly by a kind of semi-conducting polymer
With it is a kind of can UV crosslinkings polymer composition, in addition can by adding other additives, make the ink that the disclosure is provided into
The infiltration of upper solution can be completely cut off after film, while having certain Electronic Transport of Two Benzene, in use, pass through spin coating, blade coating, silk
Wire mark brush or inkjet printing can obtain good filming performance.
According to the disclosure in a first aspect, the organic solvent be used for dissolve poly- (vinyl cinnamate), it is poly- that (9,9- bis- is pungent
Base fluorenes) and polymeric additive.There is organic solvent suitable boiling point, viscosity and surface tension to be that by inkjet printing
Key, and simultaneously not all solvent can reach very good effect.The present inventor has found that boiling point is no more than by many experiments
200 DEG C of organic solvent, further, at least one in toluene, methyl phenyl ethers anisole, DMF or chlorobenzene,
The organic solvent of preferably toluene and/or methyl phenyl ethers anisole has good ink jet printing performance.
According to the disclosure in a first aspect, polymeric additive can play regulation and control ink viscosity and the work of surface tension
With enabling ink to form the film of good different-thickness on active layer.The polymeric additive can be polyphenyl second
Alkene and/or polymethyl methacrylate.The weight average molecular weight of polymeric additive is 10000-50000, if polymeric additive
Weight average molecular weight it is too low, ink viscosity not enough, surface tension is too low, then ink-jet effect is bad；If polymeric additive weight is equal
Molecular weight is too high, system viscosity increase, then printer head can be caused to block, it is impossible to ink-jet.
It is described to be used as the poly- of photocrosslinkable polymer according to the disclosure in a first aspect, inventor has found by many experiments
The concentration of (vinyl cinnamate) (Poly (vinyl cinnamate), PVCN) is 5-40mg/mL, is used as conducting polymer
Poly- (9,9- dioctyl fluorene) (Poly (9,9-di-n-octylfluorenyl), PFO) concentration is 0.5-5mg/mL, and the two weight
Amount is than being preferably (5-20)：When 1, cushion of good performance can be just obtained.Can be in purple using the film prepared by the ink
It is crosslinked under outer light irradiation, and effectively stops the infiltration of upper electrode ink.
According to the disclosure in a first aspect, viscosity and surface tension are the important performance indexes of decision ink jet quality.
If the viscosity of ink is excessive, ink can not spray, so as to block shower nozzle；If ink viscosity is too small, occur drop ink or
Drop down the phenomenon of ink.If the surface tension of ink is excessive, ink can not equally spray or ink-jet after ink be not easy infiltrate base
Bottom, if the surface tension of ink is too small, occurs satellite ink droplet, drop ink or the phenomenon for dropping down ink.The disclosed invention people passes through
Experiment finds that the viscosity and surface tension of ink are within the scope of following, and ink jetting quality is more excellent：The range of viscosities of ink is preferably
2-30 centipoises (CPS), are more preferably 3-5 centipoises, when ink viscosity be less than 2 centipoise when, have maximum probability occur drop ink or
The phenomenon of ink is dropped down, when ink viscosity is more than 20 centipoise, has maximum probability the phenomenon for blocking shower nozzle occur.In addition, surface tension is excellent
Elect 20-40 dynes per centimeters (dynes/cm), more preferably 25-35 dynes per centimeters as.When the surface tension of ink reaches less than 20
Because/centimetre when, there is maximum probability the phenomenon of satellite ink droplet occur, when ink surface tension be more than 40 dynes per centimeter when, have probably
Rate occur can not ink-jet situation.
There is provided a kind of ink for being used to make flexible organic light emission electrochemical cell cushion for disclosure second aspect
Preparation method, including：Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes) and polymeric additive and organic solvent is mixed
Close, obtain ink；Wherein, the concentration of poly- (vinyl cinnamate) is 5-40mg/mL, poly- (9,9- dioctyl fluorene) in the ink
Concentration be 0.5-5mg/mL, the polymeric additive account for the ink weight ratio be 1-10 weight %；Preferably, it is described
The concentration of (vinyl cinnamate) poly- in ink is 10-20mg/mL, and the concentration of poly- (9,9- dioctyl fluorene) is 1-3mg/mL, institute
State polymeric additive and account for the weight ratio of the ink for 3-6 weight %, the weight average molecular weight of the polymeric additive is
10000-50000。
According to the second aspect of the disclosure, the organic solvent is for dissolving poly- (vinyl cinnamate), poly- (9,9- bis- is pungent
Base fluorenes) and polymeric additive.There is organic solvent suitable boiling point, viscosity and surface tension to be that by inkjet printing
Key, and simultaneously not all solvent can reach very good effect.Inventor has found organic solvent boiling point by many experiments
No more than 200 DEG C.Further, organic solvent with good ink jet printing performance can be selected from toluene, methyl phenyl ethers anisole, N,
At least one in dinethylformamide or chlorobenzene, preferably toluene and/or methyl phenyl ethers anisole.
According to the second aspect of the disclosure, polymeric additive can play regulation and control ink viscosity and the work of surface tension
With enabling ink to form the film of good different-thickness on active layer.The polymeric additive can be selected from poly-
At least one in styrene or polymethyl methacrylate, preferably polystyrene and/or polymethyl methacrylate.Polymerization
The weight average molecular weight of thing additive is 10000-50000, if the weight average molecular weight of polymeric additive is too low, ink viscosity is not
Enough, surface tension is too low, then ink-jet effect is bad；If polymeric additive weight average molecular weight is too high, system viscosity increase then can
Printer head is caused to block, it is impossible to ink-jet.
According to the second aspect of the disclosure, inventor has found by many experiments, described to be used as the poly- of photocrosslinkable polymer
The concentration of (vinyl cinnamate) (Poly (vinyl cinnamate), PVCN) is 5-40mg/mL, is used as conducting polymer
When the concentration of poly- (9,9- dioctyl fluorene) (Poly (9,9-di-n-octylfluorenyl), PFO) is 0.5-5mg/mL, and two
Person's weight is than being preferably (5-20)：When 1, cushion of good performance can be just obtained.Can using the film prepared by the ink
It is crosslinked under ultraviolet light, and effectively stops the infiltration of upper electrode ink.
According to the second aspect of the disclosure, methods described can also include：By poly- (vinyl cinnamate), poly- (9,9- bis-
Octyl group fluorenes) and polymeric additive mixed with organic solvent after be stirred successively, ultrasound and filtering.Stirring, ultrasound and filtering
It is technology well-known to those skilled in the art, stirring and ultrasound are used for each component in dispersible ink, reduce precipitation, mixing time
Can be with 0.5-1 hours, supersonic frequency can be 20-40kHz, and the time can be 1-10min；Filtration treatment is used to filter in ink
Sediment fraction, prevent printer head to be blocked and improve printing effect, its filtering accuracy can be 0.1-0.5 microns.
The disclosure third aspect makes flexible organic hair there is provided the ink that a kind of use disclosure first aspect is provided
The method of photoelectrochemical cell cushion, including：Make ink film；Wherein, it is described make ink film mode be selected from
At least one in inkjet printing, silk-screen printing, spin coating or blade coating；Gained ink film, which is placed under ultraviolet light, makes its internal hair
Raw cross-linking reaction.
According to the third aspect of the disclosure, preferably ink film is heated and removed after organic solvent, under uv lamps
Irradiation crosslinking, general irradiation 5-20min can just reach good cross-linking effect, without in vacuum drying chamber, nitrogen glove box
Etc. removing residual solvent in particular/special requirement environment, it is not required that post-processed under the light conditions such as infrared lamp and laser.
According to the third aspect of the disclosure, if making ink film by scratching, change concentration and blade coating condition is (such as fast
Degree, baseplate temp and blade coating height etc.) it can obtain the ink film that thickness is 50nm-1 μm；If it is thin to make ink by spin coating
Film, changes concentration and spin coating rotating speed can obtain the ink film that thickness is 20-300nm.
According to the third aspect of the disclosure, it can adopt and prepare cushion using the ink of the disclosure in various manners, in order to
Reach the purpose for freely patterning preparation that cushion is realized in the case of without mask plate, the mode of the making ink film
Preferably inkjet printing and/or silk-screen printing, more preferably lasting inkjet printing, voltage during ink-jet are preferably more than 20V,
Sprayed film thickness is generally 300nm-1 μm.
There is provided a kind of flexible organic light emission electricity of making provided by the disclosure third aspect for disclosure fourth aspect
Flexible organic light emission electrochemical cell cushion made by the method for chemical cell cushion.
According to the fourth aspect of the disclosure, the mode according to inkjet printing or silk-screen printing prepares cushion, the disclosure
The pattern for the cushion that fourth aspect is provided can with unrestricted choice, pattern accuracy and definition ratio in the prior art by spin coating or
Cushion prepared by knife coating procedure is more preferable.
In addition to preparing cushion, ink described in the disclosure can also make in paint coating as coating outside cross-linking agent
With can be also used for preparing the crosslinkable semiconductor material thin film in wearable device.
The disclosure will be further illustrated by embodiment below, but the disclosure is not therefore any way limited.
Unless otherwise specified, disclosure agents useful for same be it is commercially available, commercial grades difference do not influence to use.In the embodiment of the present disclosure
Ink viscosity is tested by the portable viscosity apparatus of U.S. Rheosense microVISC, and surface tension is full-automatic using BZY-101
Surface tension instrument is tested by platinum plate method, and test temperature is 20 DEG C.
Embodiment 1
Weigh 20mg poly- (vinyl cinnamate) and 2mg poly- (9,9- dioctyl fluorene) and be transferred in reagent bottle, add 1mL
Toluene, adds the polystyrene of 2 weight % ink weight, magnetic agitation is after 1 hour, and ultrasound 5min, is then used under 40kHz
0.22 μm of filtering head filtering, obtains ink, concrete composition is shown in Table 1.
Ink is fitted into print cartridge, can be stablized with ink-jet printer and spray ink film, cause can be formed after UV crosslinkings
Close crosslinked film, can play a part of stopping upper strata ink bleed, the specific performance of ink is shown in Table 2, using the ink system
The cushion of work can reach the standard that uses, and can not only obstruct the infiltration of silver inks water but also can transmit electronics.
Embodiment 2-6
Embodiment 2-6 preparation process is substantially the same manner as Example 1, and concrete composition is shown in Table 1, and the specific performance of ink is shown in Table
2, the cushion that the ink prepared using embodiment 2-6 is made can reach the standard that uses, and can both obstruct the infiltration of silver inks water
Electronics can be transmitted again.
The preferred embodiment of the disclosure described in detail above, still, the disclosure are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the disclosure, a variety of simple variants can be carried out with technical scheme of this disclosure, this
A little simple variants belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the disclosure to it is various can
The combination of energy no longer separately illustrates.
In addition, can also be combined between a variety of embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought, it should equally be considered as disclosure disclosure of that.
Table 1
Table 2
| Embodiment | Viscosity, centipoise | Surface tension, dynes per centimeter | Ink-jet situation |
| Embodiment 1 | 2.3 | 30.1 | Well |
| Embodiment 2 | 2.1 | 28.9 | Well |
| Embodiment 3 | 3.5 | 27.2 | Well |
| Embodiment 4 | 4.1 | 30.5 | Well |
| Embodiment 5 | 4.5 | 35.0 | Well |
| Embodiment 6 | 4.6 | 35.1 | Well |
Claims (13)
1. a kind of ink for being used to make flexible organic light emission electrochemical cell cushion, including：
Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorenes), polymeric additive and organic solvent；
Wherein, the concentration of poly- (vinyl cinnamate) is 5-40mg/mL in the ink, and the concentration of poly- (9,9- dioctyl fluorene) is
0.5-5mg/mL, the weight ratio that the polymeric additive accounts for the ink is 1-10 weight %, the polymeric additive
Weight average molecular weight is 10000-50000.
2. ink according to claim 1, wherein, the organic solvent is selected from toluene, methyl phenyl ethers anisole, N, N- dimethyl methyls
At least one in acid amides or chlorobenzene, the polymeric additive is polystyrene and/or polymethyl methacrylate.
3. ink according to claim 1 or 2, wherein, the organic solvent is toluene and/or methyl phenyl ethers anisole.
4. ink according to claim 1, wherein, poly- (vinyl cinnamate) and the weight of poly- (9,9- dioctyl fluorene)
Amount is than being (5-20)：1.
5. a kind of preparation method for being used to make the ink of flexible organic light emission electrochemical cell cushion, including：
Poly- (vinyl cinnamate), poly- (9,9- dioctyl fluorene) and polymeric additive are mixed with organic solvent, ink is obtained；
Wherein, the concentration of poly- (vinyl cinnamate) is 5-40mg/mL in the ink, and the concentration of poly- (9,9- dioctyl fluorene) is
0.5-5mg/mL, the weight ratio that the polymeric additive accounts for the ink is 1-10 weight %, the polymeric additive
Weight average molecular weight is 10000-50000.
6. preparation method according to claim 5, wherein, the organic solvent is selected from toluene, methyl phenyl ethers anisole, N, N- diformazans
At least one in base formamide or chlorobenzene, the polymeric additive is polystyrene and/or polymethyl methacrylate.
7. the preparation method according to claim 5 or 6, wherein, the organic solvent is toluene and/or methyl phenyl ethers anisole.
8. preparation method according to claim 5, wherein, poly- (vinyl cinnamate) and poly- (9,9- dioctyl fluorene)
Weight ratio be (5-20)：1.
9. preparation method according to claim 5, methods described also includes：By poly- (vinyl cinnamate), poly- (9,9- bis-
Octyl group fluorenes) and polymeric additive mixed with organic solvent after be stirred successively, ultrasound and filtering.
10. preparation method according to claim 9, wherein, the time of the stirring is 0.5-1 hours, described ultrasonic
Time is 1-10min, and supersonic frequency is 20-40kHz, and the precision of the filtering is 0.1-0.5 μm.
11. the ink in a kind of use claim 1-4 described in any one makes flexible organic light emission electrochemical cell buffering
The method of layer, including：
Make ink film；Wherein, the mode for making ink film is selected from inkjet printing, silk-screen printing, spin coating and scraped
At least one in painting；
Gained ink film, which is placed under ultraviolet light, to be made to crosslink reaction inside it.
12. the method according to claim 11 for making flexible organic light emission electrochemical cell cushion, wherein, the system
The mode for making ink film is inkjet printing and/or silk-screen printing.
13. made by the method for the flexible organic light emission electrochemical cell cushion of making according to claim 11 or 12
Flexible organic light emission electrochemical cell cushion.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100127269A1 (en) * | 2008-11-26 | 2010-05-27 | Palo Alto Research Center Incorporated | Method and structure for establishing contacts in thin film transistor devices |
| CN101872686A (en) * | 2010-06-22 | 2010-10-27 | 彩虹集团公司 | Method for preparing dye-sensitized solar cell module |
| CN106058067A (en) * | 2016-08-19 | 2016-10-26 | 深圳市华星光电技术有限公司 | Organic electroluminescence diode and preparation method of cavity transmission layer thereof |
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2017
- 2017-04-19 CN CN201710258766.3A patent/CN106947321B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100127269A1 (en) * | 2008-11-26 | 2010-05-27 | Palo Alto Research Center Incorporated | Method and structure for establishing contacts in thin film transistor devices |
| CN101872686A (en) * | 2010-06-22 | 2010-10-27 | 彩虹集团公司 | Method for preparing dye-sensitized solar cell module |
| CN106058067A (en) * | 2016-08-19 | 2016-10-26 | 深圳市华星光电技术有限公司 | Organic electroluminescence diode and preparation method of cavity transmission layer thereof |
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