CN110294967A - Ink and preparation method thereof - Google Patents
Ink and preparation method thereof Download PDFInfo
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- CN110294967A CN110294967A CN201810236834.0A CN201810236834A CN110294967A CN 110294967 A CN110294967 A CN 110294967A CN 201810236834 A CN201810236834 A CN 201810236834A CN 110294967 A CN110294967 A CN 110294967A
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- ink
- magnetic
- carrier transmission
- transmission material
- inorganic semiconductor
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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
-
- 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
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- 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
- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
-
- 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
-
- 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
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
Abstract
The present invention provides a kind of inks, are the following component including following weight percentage: magnetic carrier transmission material 0.01-30.0% in terms of 100% by the total weight of the magnetism carrier transmission material ink；Organic solvent 70-99.9%；The magnetism carrier transmission material is the magnetic carrier transmission material of core-shell structure, wherein the kernel of the core-shell structure is magnetic nanoparticle, and shell is carrier transmission material, and the carrier transmission material is inorganic semiconductor material.
Description
Technical field
The invention belongs to field of display technology more particularly to a kind of ink and preparation method thereof.
Background technique
Light emitting diode with quantum dots (Quantum Dot Light Emitting Diodes QLED) is received based on inorganic
The luminescent device of the quanta point material of meter Jing, since it is with Wavelength tunable, emission spectrum is narrow, stability is high, electroluminescent amount
The advantages that sub- yield is high, becomes the contenders of next-generation display technology.
In QLED device, usual transportable hole reaches luminescent layer through hole injection, transport layer by anode, and with by cathode
The electronics migrated through electron injection, transport layer is compounded to form exciton, and then exciton radiation-emitting photon.Carrier balance problem at
An important factor for influence QLED device, particularly multilayered structure QLED device light emitting efficiency.It should be noted, however, that mistake
More holes or electronics can all generate three particIe systems to cause generate Exciton quenching, thus reduce device light emitting efficiency and
Stability.Therefore, in different type device, change carrier mobility, improving carrier injection balance is to improve device effect
The effective ways of rate and stability.
In recent years, due to inkjet printing technology have many advantages, such as high-precision, without Mask, untouchable, print on demand and
It gets more and more people's extensive concerning.Phototube is wherein made based on the functional material of solution and advanced ink jet printing device
Part can effectively improve stock utilization, reduce cost and improve production efficiency.But currently, there is also a series of problems for the technology
Have to be solved.Its key problem is ink jet printing device to the more demanding of ink, including ink chemistry, physical property,
Configuration method, printing Pre-and Post-processing etc., this brings huge challenge to ink formulation.Current quantum dot ink is through ink-jet
The quantum dot light emitting layer carrier of printing preparation injects imbalance, and then influences device performance.In addition, ink is to QLED device
Whether other structures cause change physically or chemically and damage also to can not be ignored.
Summary of the invention
Ink and preparation method thereof, it is intended to carrier injection imbalance in existing LED device is solved, thus shadow
The problem of the problem of luminous efficiency and stability of Chinese percussion instrument part.
For achieving the above object, The technical solution adopted by the invention is as follows:
One aspect of the present invention provides a kind of ink, and the total weight with the magnetism carrier transmission material ink is
100% meter, the following component including following weight percentage:
Magnetic carrier transmission material 0.01-30.0%；
Organic solvent 70-99.9%；
The magnetism carrier transmission material is the magnetic carrier transmission material of core-shell structure, wherein the nucleocapsid knot
The kernel of structure is magnetic nanoparticle, and shell is carrier transmission material.
Another aspect of the present invention provides a kind of preparation method of ink, comprising the following steps:
Each component is provided according to the formula of above-mentioned ink；
Disperse the magnetic carrier transmission material in the organic solvent, or by magnetic carrier transmission material and
Surfactant-dispersed obtains ink in organic solvent.
Another aspect of the invention provides a kind of preparation method of film, comprising the following steps:
Ink is prepared according to the method described above；
The inkjet printing deposited ink on carrier obtains magnetic carrier film by being dried.
Ink provided by the invention adds magnetic nanoparticle, and the carrier transport in carrier transmission material
Material is coated on magnetic nanoparticle surface and forms core-shell structure, and disperses in organic solvent, so that the ink is through ink-jet
Contain magnetic nanoparticle in the magnetic carrier film of printing-filming.Since there are long-range orders for the magnetic nanoparticle
Magnetic moment, carrier moving will receive magneton, phonon and iron magnetic non-magnetic interface scattering effect, to change carrier blocking layers
Carrier mobility, and then improve device in carrier injection balance.When the magnetic quantum dot film is for shining two
When in pole pipe especially QLED device, the carrier injection balance that can be effectively improved in device, and then improve device efficiency and
Stability.Further, under the premise of with magnetic nanoparticle and carrier transmission material collectively as solute, the present invention is mentioned
The ink of confession makes the ink containing magnetic material of suitable inkjet printing by control ink composition.And inkjet printing is completed
Afterwards, by applying external magnetic field to magnetic quantum dot into pinning effect, and then " coffee ring effect " is eliminated, improves film morphology,
Promote device performance.
The preparation method of ink provided by the invention need to only disperse magnetic carrier transmission material in organic solvent,
It is easy to operate easily-controllable or by the sub- transmission material of magnetic flow and surfactant-dispersed in organic solvent, it does not need harsh
Condition, it can be achieved that produce in enormous quantities.
The preparation method of film provided by the invention, only need to be by magnetic nanoparticle and carrier transmission material organic molten
It is fully dispersed in agent, ink is made, and then progress inkjet printing, drying can be obtained on carrier, method is simple, it is easy to accomplish
Standardization control.
Specific embodiment
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
The meaning of " plurality " is two or more, unless otherwise specifically defined.
Carrier will receive the scattering process power of magnetic force and magneton and make its motion profile when moving in magnetic field
It deflects, to change carrier mobility.In magnetic material, since there are the magnetic moment of long-range order, carrier movings
It will receive magneton, phonon and iron magnetic non-magnetic interface scattering effect, to change carrier mobility.Therefore, the present invention is implemented
In example, change this feature of carrier mobility using magnetic material, by the way that (electronics is infused in traditional carrier transmission material
Enter/transmission material or hole injection/transmission material), introduce magnetic material in electrode material (cathode material or anode material), into
And it is configured to the mode of ink, to change carrier mobility, improve the carrier in light emitting diode especially QLED device
Injection balance, and then improve device luminescent properties and stability.
Specifically, action principle of the magnetic material as aid functional material in light emitting diode such as QLED device are as follows:
To the carrier functional layer containing magnetic material or the electrode containing magnetic material preparation light emitting diode such as
After QLED device applies electric field, carrier is moved by electric field action power along direction of an electric field, but part carrier will receive at this time
Impurities of materials or defect scattering, phon scattering act on and change motion profile, to cause the change of carrier mobility.Together
When, the factors such as this variation size and temperature, impurity state defects count are closely related.When there are externally-applied magnetic field, carrier exists
It will receive the effect of Lorentz force in motion process and make carrier moving trajectory deflection, to form electric field in bilateral summation
(Hall effect) causes the change of carrier mobility.And for magnetic material, spontaneous existing magneton can be to carrier
Magnon scattering, the deflection to cause motion profile are generated, so as to cause carrier mobility change.In magnetic material due to
Existing a variety of scattering processes cause carrier mobility to change up to as many as 2~3 orders of magnitude.Based on this, light emitting diode
As in QLED device due to carrier mobility difference existing for carrier inject unbalanced problem, can be by shining two
Magnetic material is introduced in pole pipe such as QLED device to adjust, and so as to improve carrier injection balance, improves device efficiency.
Specifically, when magnetic material with particle size distributions in carrier functional layer or electrode, apply outfield after particle
It is magnetized, magnetic moment is arranged along magnetic direction, and the magnetic moment orientation for removing externally-applied magnetic field magnetic material at this time is still constant.It is thin
The arrangement of magnetic moment direction changes with the variation in outfield in film, and carrier mobility also changes correspondingly, therefore can pass through
Apply outfield to improve carrier injection balance, optimized device performance.
In view of this, on the one hand the embodiment of the present invention provides a kind of ink, with the magnetism carrier transmission material ink
The total weight of water is 100% meter, the following component including following weight percentage:
Magnetic carrier transmission material 0.01-30.0%；
Organic solvent 70-99.9%；
The magnetism carrier transmission material is the magnetic carrier transmission material of core-shell structure, wherein the nucleocapsid knot
The kernel of structure is magnetic nanoparticle, and shell is carrier transmission material.
Ink provided in an embodiment of the present invention adds magnetic nanoparticle, and the current-carrying in carrier transmission material
Sub- transmission material is coated on magnetic nanoparticle surface and forms core-shell structure, and disperses in organic solvent, so that the ink
Contain magnetic nanoparticle in magnetic carrier film through inkjet printing film forming.Since there are long-ranges for the magnetic nanoparticle
Orderly magnetic moment, carrier moving will receive magneton, phonon and iron magnetic non-magnetic interface scattering effect, to change carrier
The carrier mobility of transport layer, and then improve the carrier injection balance in device.When the magnetic quantum dot film is used for
When in light emitting diode especially QLED device, the carrier injection balance that can be effectively improved in device, and then improve device
Efficiency and stability.Further, under the premise of with magnetic nanoparticle and carrier transmission material collectively as solute, this
The ink that inventive embodiments provide makes the ink containing magnetic material of suitable inkjet printing by control ink composition.And
After the completion of inkjet printing, by applying external magnetic field to magnetic quantum dot into pinning effect, and then " coffee ring effect " is eliminated, changed
Kind film morphology, promotes device performance.
Ink provided in an embodiment of the present invention, the core-shell structure formed with magnetic nanoparticle and carrier transmission material
Magnetic carrier transmission material is equipped with organic solvent as solute.The magnetic carrier transmission material of the core-shell structure can
In organic solvent, the ink properties of preparation can satisfy the production requirement of inkjet printing printing technology for dispersion, and at
It can be by additional condition (magnetic field, electric field, temperature) come controlled material performance after film.
Specifically, the magnetism carrier transmission material is the magnetic carrier transmission material with core-shell structure, it is described
The kernel of core-shell structure is magnetic nanoparticle, and shell is carrier transmission material.Thus obtained ink, through inkjet printing at
After film, the function of carrier transport is played as the carrier transmission material of shell；And the magnetic nanoparticle energy as kernel
Under the action of externally-applied magnetic field, the movement of carrier will receive magneton, phonon and iron magnetic non-magnetic interface scattering effect, current-carrying
Transport factor is improved, and carrier injection balance improves.It is worth noting that, in the embodiment of the present invention, due to the transmission
Material realizes transfer function, and therefore, when forming core-shell structure magnetic carrier transmission material, carrier transmission material is as shell
The magnetic nanoparticle surface is coated on (if the carrier transmission material, as kernel, and magnetic nanoparticle is as outer
Shell, the then transmission performance that carrier transmission material can not bring into normal play).
In the embodiment of the present invention, function auxiliary material of the magnetic nanoparticle as equilbrium carrier migration performance.
Preferably, as the magnetic nanoparticle of kernel be selected from iron simple substance, ferriferous oxide, ferroalloy, cobalt simple substance, cobalt/cobalt oxide,
At least one of cobalt alloy, nickel simple substance, nickel oxide, nickel alloy.Preferred magnetic nanoparticle, the current-carrying formed after film forming
Sub- transmission material for light emitting diode especially QLED device when, under magnetic fields, can more effectively improve carrier
Mobility improves carrier injection balance, to improve device luminescent properties.It is further preferred that the magnetic nanoparticle
Selected from Fe3O4、Fe2O3, at least one of NiO, CoO, FeCo, FeCr.
Specifically, the magnetic nanoparticle is selected according to the type of specific carrier transmission material.Preferably,
The carrier transmission material is inorganic semiconductor material, including N-type inorganic semiconductor material and p-type inorganic semiconductor material.
As an implementation, the carrier transmission material is electron transport material, and the electron transport material is preferably N at this time
Type inorganic semiconductor material.When the carrier transmission material is electron transport material, it is preferred that the magnetic nanoparticle choosing
From Fe3O4、Fe2O3, at least one of NiO, CoO, FeCo, FeCr.As another embodiment, the carrier transport
Material is hole mobile material, at this point, N-type inorganic semiconductor material may be selected for the hole mobile material or p-type is inorganic partly leads
Body material.Specifically, when selecting N-type inorganic semiconductor material as hole mobile material, corresponding magnetic oxide material
Material need to select N-type semiconductor；It is corresponding magnetic oxygenated when selecting p-type inorganic semiconductor material as hole mobile material
Object material need to select P-type semiconductor, to improve the transporting of carrier under the premise of the basic transmission performance in guarantee hole
Energy.When the carrier transmission material is electron transport material, it is preferred that the magnetic nanoparticle is selected from Fe3O4、Fe2O3、
At least one of NiO, CoO.
In the embodiment of the present invention, carrier of the carrier transmission material as basic function material, after assigning film forming
Transmission film carrier transmission performance.The carrier transport that the material of the carrier transmission material constructs according to specific needs is thin
Film (hole transport film or electron-transport film) is determined, i.e., magnetic carrier transmission material is used for transmission electronics or hole,
Determined by the property of carrier transmission material, it can be using conventional carrier transmission material.As an implementation, described
Carrier transmission material is electron transport material, specifically, the electron transport material is N-type inorganic semiconductor material, the N
Type inorganic semiconductor material is preferably N-type transition metal oxide nano particle, is particularly preferred as ZnO, TiO2、SnO2In extremely
Few one kind.As another embodiment, the carrier transmission material is hole mobile material, and the hole mobile material is
N-type inorganic semiconductor material or p-type inorganic semiconductor material, the N-type inorganic semiconductor material are selected from N-type transiting metal oxidation
Object nano particle, the p-type inorganic semiconductor material is selected from p-type transition metal inorganic semiconductor nano particle, specifically, described
N-type transition metal oxide nano particle includes but is not limited to V2O5、WO3、MoO3, the p-type transition metal inorganic semiconductor receives
Rice grain includes but is not limited to MoO2, SnO, mix the MoO after sulphur modification3。
In the embodiment of the present invention, it is preferred that the partial size of the kernel is 1-15nm, more preferably 10nm.The kernel
Partial size is too small, and it is difficult to synthesize, and material homogeneity is difficult to control；If the partial size of the kernel is excessive, obtained film table
Surface roughness is larger, is unfavorable for the deposition of further next functional layer, and the electric leakage of thus obtained film layer is big, under photoelectric properties
Drop.Preferably, the shell with a thickness of 1-12nm, more preferably 10nm.If the thickness of the shell is excessively thin, carrier is passed
Defeated material is difficult to coat the magnetic nanoparticle completely, and the carrier transmission performance of carrier transmission material is caused to decline；If
The thickness of the shell is blocked up, on the one hand, is unfavorable for the limitation of particle size, the surface roughness of the film resulted in increases
Add；On the other hand, it is unfavorable for the magnetic nanoparticle and plays its function.In the embodiment of the present invention, carrier transmission material packet
The magnetic carrier transmission material for overlaying on the core-shell structure of magnetic nanoparticle surface formation has superparamagnetism, and in room temperature
Under the conditions of (10-30 DEG C), the saturation magnetization of the magnetism carrier transmission material is 1-150emu/g.
In the embodiment of the present invention, the magnetism carrier transmission material accounts for the 0.01%-30.0% of the ink total weight,
To obtain surface tension and the suitable ink of viscosity, specific weight percentage can for 0.01%, 0.2%, 0.5%,
0.8%, 1.0%, 2.0%, 4.0%, 5.0%, 8.0%, 10.0%, 12.0%, 15.0%, 18.0%, 20.0%,
22.0%, the specific values content such as 25.0%, 28.0%, 30.0%.
In the embodiment of the present invention, the solvent for dispersing the magnetic carrier transmission material is organic solvent, it is preferred that
Contain alcohol organic solvent in the organic solvent, and the alcohol organic solvent accounts for the 1%- of the organic solvent total weight
90%.The alcohol organic solvent is used as the current-carrying of light emitting diode especially QLED device as ink solvent, printing-filming
When sub- film, it is possible to prevente effectively from the influence to deposited good adjacent functional layer material.Further, the alcohols is organic
Solvent is selected from lower alcohol, higher alcohol and lower alcohol, higher alcohol combines the mixed solvent to be formed, wherein the lower alcohol is carbon
Monohydric alcohol of the atomicity between 1-5, the higher alcohol is the polyalcohol that carbon atom number is more than or equal to 4, such as dihydric alcohol, trihydroxylic alcohol
Deng.Specifically, the lower alcohol include but is not limited to methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, 2- butanol, the tert-butyl alcohol,
At least one of 2- methyl-1-propyl alcohol, the higher alcohol include but is not limited to 1,2- butanediol, 1,3-BDO, Isosorbide-5-Nitrae-fourth
At least one of glycol, 2,3- butanediol, 1,5- pentanediol, glycerine, 1,2,4- butantriol, 1,2,3- butantriol.
In the embodiment of the present invention, the organic solvent accounts for the 70%-99% of the ink total weight, and specific weight percent contains
Amount can be the specific values content such as 70%, 75%, 80%, 85%, 90%, 95%, 99%.
In the embodiment of the present invention, due to having stronger interaction between the magnetic nanoparticle, the magnetism is received
It is easy to reunite due to attracting each other between rice grain, and the organic solvent for being provided purely for dissolution solute can not effectively weaken magnetism
Intergranular interaction force cannot make magnetic nanoparticle evenly dispersed under larger concentration.Therefore, in order to better disperse
The magnetic nanoparticle prevents from reuniting between the magnetic nanoparticle due to attracting each other, it is preferred that in the ink
Middle addition surfactant contains surfactant in that is, described ink.It is further preferred that the surfactant is alcohols
Nonionic surface active agent.The alcohols nonionic surface active agent can reduce magnetic nanoparticle surface with it is organic molten
Interfacial tension between agent molecule, improves the wettability of magnetic nanoparticle, to enhance the dispersibility of magnetic nanoparticle.Together
When, since the interaction between alcohols nonionic surface active agent and magnetic nanoparticle is electroneutral, and alcohols is non-
Ionic surfactant belongs to organic matter, thus the magnetic nanoparticle of alcohols nonionic surface active agent cladding can lead to
It crosses the spacing increased between adjacent magnetic nano particle and effectively weakens intergranular attraction, so that it is steady to make it have dynamics
It is qualitative, it can be preferably scattered in organic solvent altogether with carrier transmission material.
Specifically, the preferred glycol ester of the alcohols nonionic surface active agent, glyceride, neopentyl type polyol ester
At least one of equal polyalcohols, but not limited to this.
It is in terms of 100% by the total weight of the ink, the weight percent of the surfactant contains in the embodiment of the present invention
Amount is 0.01%-5.0%, specific weight percentage can for 0.01%, 0.1%, 0.2%, 0.5%, 0.8%, 1.0%,
2.0%, the specific values content such as 4.0%, 5.0%.If the content of the surfactant is too low, limited, Bu Nengyou is acted on
Effect disperses the magnetic nanoparticle, is easy to reunite between the magnetic nanoparticle；If the content mistake of the surfactant
Height then will affect ink overall viscosity and surface tension, be unfavorable for inkjet printing.
Ink provided in an embodiment of the present invention has preferable surface tension and viscosity, the printing suitable for ink-jet apparatus.Tool
Body, surface tension when ink room temperature (10-30 DEG C) is 10-50dynes/cm, is preferably controlled in 28-42dynes/
cm；Viscosity when ink room temperature (10-30 DEG C) is 1-18cP, is preferably controlled in 10-12cP.
Ink provided in an embodiment of the present invention can be prepared by following methods.
On the other hand the embodiment of the present invention provides a kind of preparation method of ink, comprising the following steps:
S01. each component is provided according to the formula of above-mentioned ink；
S02. it disperses the magnetic carrier transmission material in the organic solvent, or by magnetic carrier transport material
Material and surfactant-dispersed obtain ink in organic solvent.
The preparation method of ink provided in an embodiment of the present invention need to only disperse magnetic carrier transmission material in organic molten
It is easy to operate easily-controllable in agent, or by the sub- transmission material of magnetic flow and surfactant-dispersed in organic solvent, it does not need
Harsh condition is, it can be achieved that produce in enormous quantities.
Specifically, in above-mentioned steps S01, the formula of the ink, each component ratio, material and its preferred situation are for example above
Described, in order to save length, details are not described herein again.
In above-mentioned steps S02, disperse the magnetic carrier transmission material in organic solvent, or magnetic flow is passed
Defeated material and surfactant-dispersed carry out decentralized processing in organic solvent.Discrete form is unrestricted, can be used and stirs
The mode of mixing is realized.Table is added after the dispersion in organic solvent of magnetic carrier transmission material as a kind of specific embodiment
Face activating agent has the distributed ink of appropriate surface tension to get arriving.
Another further aspect of the embodiment of the present invention provides a kind of preparation method of film, comprising the following steps:
E01. ink is prepared according to the method described above；
E02. the inkjet printing deposited ink on carrier obtains magnetic carrier film by being dried.
The preparation method of film provided in an embodiment of the present invention, only need to be by magnetic carrier transmission material in organic solvent
It is fully dispersed, ink is made, and then progress inkjet printing, drying can be obtained on carrier, method is simple, it is easy to accomplish standard
Change control.
The method that above-mentioned steps E01 prepares ink is as described above, and in order to save length, details are not described herein again.
In above-mentioned steps E02, by selecting suitable ink-jet printer to carry out inkjet printing, in deposited on supports ink,
Then solvent flashing is dried to the ink and obtains magnetic carrier film.Specifically, the inkjet printing is preferred
It is realized using piezoelectric ink jet printing or thermal inkjet-printing.During the drying process is heating drying, cooling and drying, is dried under reduced pressure
It is at least one.As an implementation, individually using heating drying, cooling and drying, one of be dried under reduced pressure and to be dried
Processing.As another embodiment, dry using heating and be dried under reduced pressure or cooling and drying and be dried under reduced pressure place is dried
Reason.Preferably, the dry temperature of the heating is 60-280 DEG C, time 0-30min；Preferably, the temperature of the cooling and drying
Degree is 0-20 DEG C；Preferably, the vacuum degree of the drying process is 1 × 10-6Torr is to normal pressure.It is suitable to be dried mode,
It can guarantee the matrix knot for depositing carrier transport under the premise of efficiently removing the organic solvent, surfactant
Structure is not damaged.
The magnetic carrier transport dry film formed through inkjet printing, thickness is preferably 20-80nm；Further, through ink-jet
The magnetic carrier transport thickness of dry film that printing is formed is 30-50nm.
It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of preparation method of ink, comprising the following steps:
By the Fe of 0.1g3O4By be ultrasonically treated 1h be scattered in the ethyl alcohol of 30ml, 20ml deionized water mixed solution in,
90 DEG C are heated to, the triethanolamine of 1.6mol/L and the Zn (Ac) of 0.02mol/L are added after 10min2·2H2O solution, and continue
1h is stirred at 90 DEG C, is collected brown product and is collected and clean to obtain kernel to be Fe with deionized water3O4, shell be ZnO nucleocapsid
Structural material (Fe3O4@ZnO)。
Take the Fe of 0.1g3O4@ZnO nano particle is scattered in the bromine of the deionized water comprising 80ml, 0.30g/0.823mmol
Change hexadecyl trimethylamine, the concentrated gas liquor solution of 1.00g, 28wt%, in 60ml ethanol solution, and stirs 0.5h and be allowed to disperse
Uniformly.The ethylene acetate that 10ml is then added into solution is used to adjust the surface tension of solution, to obtain nucleocapsid
The compound ink of type magnetism N-type semiconductor.
Embodiment 2
A kind of QLED device, the materials described below layer including stacking gradually combination: ITO/PEDOT:PSS (poly- (3,4- ethylene two
Oxygen thiophene)-polystyrolsulfon acid)/TFB/ green QDs (quantum dot)/Fe3O4@ZnO/Al electrode.
The QLED device the preparation method comprises the following steps:
Ito substrate is provided, is sequentially prepared PEDOT:PSS layers, TFB layers, QDs layers of green on an ito substrate；
The compound ink of core-shell type magnetic N-type semiconductor prepared by embodiment 1 prints on green by ink jet printing device
On QDs layer, as electron transfer layer；
Al electrode is prepared on the electron transport layer.
Comparative example 1
A kind of QLED device, the materials described below layer including stacking gradually combination: ITO/PEDOT:PSS/TFB/ green QDs
(quantum dot)/Fe3O4@ZnO/Al electrode.
The QLED device that embodiment 2, comparative example 1 are provided carries out performance comparison: electric current is 2mA, light emitting region is
0.4m2Under conditions of, the brightness for the QLED device that comparative example 1 provides is 4800cd/m2, embodiment 2 provide QLED device it is bright
Degree is 5800cd/m2, luminance raising is 121% originally.
Embodiment 3
A kind of preparation method of ink, comprising the following steps:
There is provided the zinc naphthenate for the Zn of metal containing 10wt% that purity is 99.9%, the metal containing 12wt% that purity is 99.9%
The iron naphthenate of Fe.The iron naphthenate mixing of the 0.5mol zinc naphthenate and 0.5mol of 50ml is taken, and is thermally decomposed with flame atomizing
Method prepares the Core-shell Structure Nanoparticles (Fe@ZnO) that kernel is Fe, shell is ZnO.Wherein, flame atomizing thermally decomposes legal system
The oxygen of methane and 3.2L/min that the design parameter of standby process is set as 1.5L/min is pre-mixed as flame fuel；?
It is 1.5bar that two-phase, which sprays nozzle exit pressure in most device, is 5L/min with oxygen flow, with atomising device extract phase precursor.
Subsequent liquid phase presoma is reacted in flame atmosphere, is nucleated, growing, solidifying, being gathered into Fe@ZnO superfine nano particle.
Take Fe@ZnO of 25wt%, the ethyl alcohol of 40wt%, the glycerine of 30wt% and the glycerol triacetate of 5wt%
It is stirred evenly after mixing, obtains the compound ink of core-shell type magnetic N-type semiconductor.
Embodiment 4
A kind of QLED device, the materials described below layer including stacking gradually combination: ITO/PEDOT:PSS/TFB/ green QDs
(quantum dot)/Fe@ZnO/Al electrode.
The QLED device the preparation method comprises the following steps:
Ito substrate is provided, is sequentially prepared PEDOT:PSS layers, TFB layers, QDs layers of green on an ito substrate；
The compound ink of core-shell type magnetic N-type semiconductor prepared by embodiment 3 prints on green by ink jet printing device
On QDs layer, as electron transfer layer；
Al electrode is prepared on the electron transport layer.
The QLED device that embodiment 4, comparative example 1 are provided carries out performance comparison: electric current is 2mA, light emitting region is
0.4m2Under conditions of, the brightness for the QLED device that comparative example 1 provides is 4800cd/m2, embodiment 4 provide QLED device it is bright
Degree is 6000cd/m2, luminance raising is 125% originally.
Embodiment 5
A kind of preparation method of ink, comprising the following steps:
By the ammonium metavanadate NH of 0.2959g4VO3It is dissolved in deionized water, obtains the clear solution of glassy yellow, be added certain
The dehydrated alcohol (ethylene glycol) of amount stirs 10min.Obtained solution is moved into hydrothermal reaction kettle, it is anti-in 180 DEG C of heat preservations
Room temperature should be then cooled to for 24 hours.Gained precipitating is washed with deionized for several times, and is dried at 80 DEG C, then 500 DEG C
Lower calcining 2h, grinding obtain vanadic anhydride nano particle.Suitable vanadic anhydride nano particle is dispersed in ethyl alcohol,
Ultrasonic disperse is uniform.By a certain amount of ferric nitrate Fe (NO3)3Be dissolved in be configured in ethyl alcohol concentration be 0.1mol/L clarification it is saturating
Bright solution.Under strong stirring, by the above-mentioned Fe (NO of 1ml3)3Ethanol solution be added dropwise to 40ml V2O5Nano particle hangs
(contain 0.5mmol V in turbid2O5).Continue after stirring 2h, mixed solution is transferred in water heating kettle, 100 DEG C of hydro-thermal process
12h.After water heating kettle natural cooling, precipitating be centrifuged and remove removal of residue with ethanol washing, can be obtained kernel be Fe,
Shell is V2O5Core-shell Structure Nanoparticles (Fe@V2O5)。
Take the Fe@V of 25wt%2O5The ethyl alcohol and 30wt%1 of 42wt% is added, in 2,3- butantriols, is dripped after being uniformly dispersed
The ethylene acetate of 3wt% is added to obtain the compound ink of core-shell type magnetic N-type semiconductor.
Embodiment 6
A kind of QLED device, the materials described below layer including stacking gradually combination: ITO/PEDOT:PSS/Fe@V2O5/CdSe/
ZnO/Al。
The QLED device the preparation method comprises the following steps:
Ito substrate is provided, prepares PEDOT:PSS layers on an ito substrate；
The compound ink solution of core-shell type magnetic N-type semiconductor prepared by embodiment 5 is printed on by ink jet printing device
On Nissan layer, as hole transmission layer；
It is sequentially prepared CdSe layers, ZnO layer and Al electrode on the hole transport layer.
Comparative example 2
A kind of QLED device, the materials described below layer including stacking gradually combination: ITO/PEDOT:PSS/Fe@V2O5/CdSe/
ZnO/Al。
The QLED device that embodiment 6, comparative example 2 are provided carries out performance comparison: electric current is 2mA, light emitting region is
0.4m2Under conditions of, the brightness for the QLED device that comparative example 2 provides is 2300cd/m2, embodiment 6 provide QLED device it is bright
Degree is 2800cd/m2, luminance raising is 122% originally.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (14)
1. a kind of ink, which is characterized in that by the total weight of the ink be 100% in terms of, including following weight percentage
Following component:
Magnetic carrier transmission material 0.01-30.0%；
Organic solvent 70-99.9%；
The magnetism carrier transmission material is the magnetic carrier transmission material of core-shell structure, wherein the core-shell structure
Kernel is magnetic nanoparticle, and shell is carrier transmission material.
2. ink as described in claim 1, which is characterized in that the carrier transmission material is inorganic semiconductor material.
3. ink as described in claim 1, which is characterized in that the magnetic nanoparticle is selected from iron simple substance, ferriferous oxide, iron
At least one of alloy, cobalt simple substance, cobalt/cobalt oxide, cobalt alloy, nickel simple substance, nickel oxide, nickel alloy.
4. ink as claimed in claim 2, which is characterized in that the inorganic semiconductor material is electron transport material, described
Electron transport material is N-type inorganic semiconductor material, and/or
The magnetic nanoparticle is selected from Fe3O4、Fe2O3, at least one of NiO, CoO, FeCo, FeCr.
5. ink as claimed in claim 4, which is characterized in that the N-type inorganic semiconductor material is selected from ZnO, TiO2、SnO2。
6. ink as claimed in claim 2, which is characterized in that the inorganic semiconductor material is hole mobile material, described
Hole mobile material be N-type inorganic semiconductor material or p-type inorganic semiconductor material, and/or
The magnetic nanoparticle is selected from Fe3O4、Fe2O3, at least one of NiO, CoO.
7. ink as claimed in claim 6, which is characterized in that the N-type inorganic semiconductor material is selected from V2O5、WO3、MoO3,
The p-type inorganic semiconductor material is selected from MoO2, SnO, the MoO for mixing sulphur modification3。
8. such as the described in any item inks of claim 1-7, which is characterized in that the partial size of the kernel is 1-15nm, described outer
Shell with a thickness of 1-12nm.
9. such as the described in any item inks of claim 1-7, which is characterized in that contain surfactant in the ink, and with
The total weight of the ink is 100% meter, and the weight percentage of the surfactant is 0.01%-5.0%.
10. ink as claimed in claim 9, which is characterized in that the surfactant is alcohols non-ionic surfactant
Agent.
11. ink as claimed in claim 10, which is characterized in that the alcohols nonionic surface active agent is selected from ethylene glycol
At least one of ester, glyceride, neopentyl type polyol ester.
12. such as the described in any item inks of claim 1-7, which is characterized in that the magnetism carrier transmission material has super
Paramagnetism, and the saturation magnetization of the magnetic carrier transmission material is 1-150emu/g.
13. a kind of preparation method of ink, which comprises the following steps:
Each component is provided according to the formula of any one of the claim 1-12 ink；
It disperses the magnetic carrier transmission material in the organic solvent, or by magnetic carrier transmission material and surface
Activating agent is scattered in organic solvent, obtains ink.
14. a kind of preparation method of film, which comprises the following steps:
Ink is prepared according to claim 13 the method；
The inkjet printing deposited magnetic quantum dot ink on carrier obtains film by being dried.
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