CN107099190A - Zinc oxide base nano particle ink and electroluminescent device - Google Patents
Zinc oxide base nano particle ink and electroluminescent device Download PDFInfo
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- CN107099190A CN107099190A CN201710388619.8A CN201710388619A CN107099190A CN 107099190 A CN107099190 A CN 107099190A CN 201710388619 A CN201710388619 A CN 201710388619A CN 107099190 A CN107099190 A CN 107099190A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
Abstract
The present invention provides a kind of zinc oxide base nano particle ink, including solvent and the zinc oxide base nano particle being dispersed in the solvent, by mass percentage, in the zinc oxide base nano particle ink, the zinc oxide base nano particle accounting 0.01 20.00%, the solvent accounting 80.00 99.99%, it is characterised in that the solvent includes at least one alcohol ether ester type compound.The present invention can solve existing zinc oxide base nano particle ink and be not suitable for inkjet printing, the problem of quality of forming film is poor.Meanwhile, the invention provides a kind of electroluminescent device, its electron transfer layer is prepared by zinc oxide base nano particle ink by inkjet printing.
Description
Technical field
The present invention relates to light emitting device field, in particular to a kind of zinc oxide base nano particle ink and electroluminescent hair
Optical device.
Background technology
With the continuous progress of science and technology, display device gradually develops towards thinner, higher color domain, more stable direction.Make
For a kind of self-luminous display part, light emitting diode with quantum dots (QLED) conforms exactly to the requirement of display device of future generation,
QLED has the advantages that colour gamut height, stability are good.Zinc oxide is a kind of group Ⅱ-Ⅵ compound semiconductor of broad stopband direct band gap
Material, energy gap is 3.37eV at room temperature, is electrically showing as n-type conduction type, resistivity as little as 10-4Ω/cm.Due to
It has excellent photoelectric characteristic, and can change its position of energy band by the metallic element and ion for adulterating different.
The general of existing Zinc oxide nanoparticle electron transfer layer is prepared by spin coating mode, but spin coating mode is not suitable for
Large-size device and raw material availability are low.Inkjet technology applies to QLED show in manufacturing technology to be considered as to solve height
Cost and the effective way for realizing large area, this technology can combine functional material and advanced inkjet printing based on solution
Equipment, can improve the utilization rate and production efficiency of material, reduce manufacturing cost, improve production capacity.
Zinc oxide base nano particle has the features such as specific surface area is big, itself easily reunites, surface polarity is strong, in organic solvent
In be difficult to disperse.When zinc oxide base nano particle being printed into quantum dot light emitting layer with InkJet printing processes, there is contact angle
Greatly, the problems such as wetability is poor, has a strong impact on quality of forming film, causes easily to occur after film forming dry and cracked, orange peel, shrinkage cavity, lines etc. now
As.
Different from the luminescent layer preparation technology such as spin coating, printing, ink jet printing device requires higher to ink, for example suitably
Boiling point, viscosity, surface tension and uniform and stable scattered, bigger difficulty is brought to ink formulation.
The content of the invention
The invention provides a kind of zinc oxide base nano particle ink, to solve existing zinc oxide base nano particle ink not
The problem of being adapted to inkjet printing and poor quality of forming film.
According to an aspect of the present invention there is provided a kind of zinc oxide base nano particle ink, including solvent and dispersed
Zinc oxide base nano particle in the solvent, it is by mass percentage, described in the zinc oxide base nano particle ink
Zinc oxide base nano particle accounting 0.01-20.00%, the solvent accounting 80.00-99.99%, the solvent includes at least one
Plant alcohol ether ester type compound.
Preferably, by mass percentage, in the zinc oxide base nano particle ink, the alcohol ether ester type compound is accounted for
Compare 10.00-80.00%.
Preferably, under the conditions of 25 DEG C, the range of viscosities of the zinc oxide base nano particle ink is 1-40cP.
Preferably, under the conditions of 25 DEG C, the surface tension range of the zinc oxide base nano particle ink is 20-60mN/m.
Preferably, the boiling spread of the alcohol ether ester type compound is 50-300 DEG C.
Preferably, the alcohol ether ester type compound includes glycol methyl ether acetate, ethylene glycol ether acetate, ethylene glycol
Propyl ether acetate, ethylene glycol monomethyl ether n Propanoic acid ester, ethylene glycol ethyl ether n Propanoic acid ester, glycol propyl ether n Propanoic acid ester, ethylene glycol first
Ether isopropyl acid esters, ethylene glycol ethyl ether isopropyl acid esters, glycol propyl ether isopropyl acid esters, propylene glycol methyl ether acetate, propylene-glycol ethyl ether
Acetate, propylene glycol propyl ether acetate, propylene glycol monomethyl ether n Propanoic acid ester, propylene-glycol ethyl ether n Propanoic acid ester, propylene glycol propyl ether positive third
Acid esters, propylene glycol monomethyl ether isopropyl acid esters, propylene-glycol ethyl ether isopropyl acid esters, propylene glycol propyl ether isopropyl acid esters, diethylene glycol dimethyl ether vinegar
Acid esters, diethylene glycol ether acetate, dipropylene glycol methyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether vinegar
At least one of acid esters, dipropylene acetate.
Preferably, the solvent includes viscosity modifier, and it is 50-300 DEG C that the viscosity modifier, which includes boiling spread,
Unitary or polynary small molecular alcohol compounds, the small molecular alcohol compounds account for the zinc oxide base nano particle ink
Mass percent scope is 0.01-60.00%.
Preferably, the small molecular alcohol compounds include ethanol, propyl alcohol, butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, penta
Alcohol, isoamyl alcohol, sec-amyl alcohol, secondary isoamyl alcohol, hexanol, enanthol, octanol, nonyl alcohol, ten carbon alcohol, undecylenic alcohol, Lauryl Alcohol, 13 carbon
Alcohol, positive ethylene glycol, 1,2-PD, 1,3-PD, 1,2- butanediols, 1,3-BDO, BDO, 2,3- fourths two
Alcohol, 1,5-PD, 2- methyl -2,4- pentanediol, NPG, 2- butene-1s, 4- glycol, 2- methyl -
2,4- pentanediols, Pinacol, 2- ethyls -1,3- hexylene glycol, glycerine, BT, 1,2,6-
At least one of hexanetriol, pentaerythrite.
Preferably, the solvent includes the alkoxide compound that boiling spread is 50-300 DEG C, the alkoxide compound
The mass percent scope for accounting for the zinc oxide base nano particle ink is 0.01-60.00%.
Preferably, the alkoxide compound includes acetic acid glycol ester, propionic acid glycol ester, butyric acid glycol ester, penta
Sour glycol ester, propylene glycol acetate, propionic acid propylene glycol ester, butyric acid propylene glycol ester, valeric acid propylene glycol ester, acetic acid butanediol ester,
Propionic acid butanediol ester, butyric acid butanediol ester, valeric acid butanediol ester, acetin, diacetine, acetic acid diethylene glycol
At least one in ester, propionic acid binaryglycol ester, butyric acid binaryglycol ester, 2,2,4- trimethyl -1,3- pentanediol mono isobutyrates
Kind.
Preferably, the solvent includes alcohol ethers compound, and the alcohol ethers compound accounts for the zinc oxide base nano
The mass percent scope of grain ink is 0.01-60.00%.
Preferably, the alcohol ethers compound includes ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol propyl ether, ethylene glycol fourth
Ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propylene glycol propyl ether, propandiol butyl ether, butanediol methyl ether, butanediol ether, butanediol third
Ether, butanediol butyl ether, diethylene glycol ether, diethylene glycol dimethyl ether, diethylene glycol dimethyl ether, diethylene glycol ether, diethylene glycol two
Ether, diethylene glycol propyl ether, diethylene glycol dipropyl ether, butyl, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, two
Propylene glycol monomethyl ether, dimethyl ether, DPE, dipropylene glycol diethyl ether, dipropylene, triethylene glycol
At least one of ether, tripropylene glycol methyl ether, tripropylene glycol butyl ether.
Preferably, the solvent includes dispersant, and the dispersant includes alcamine compound or sulfur alcohol compound.
Preferably, the dispersant includes monoethanolamine, diethanol amine, triethanolamine, N methyldiethanol amine, N- ethyls two
Monoethanolamine, N- n-propyls diethanol amine, N- isopropyldiethanolamines, N- n-butyldiethanolamines, normal propyl alcohol amine, isopropanolamine,
At least one of diisopropanolamine (DIPA), butanolamine, amylalcohol amine, dithioglycol.
Preferably, the particle size range for stating zinc oxide base nano particle is 1-100nm.
Preferably, the zinc oxide base nano particle is mixed including Zinc oxide nanoparticle, metal ion mixing or oxide
Miscellaneous Zinc oxide nanoparticle.
According to another aspect of the present invention there is provided a kind of electroluminescent device, including it is negative electrode, electron transfer layer, luminous
Layer, hole transmission layer and anode, the electron transfer layer are prepared by above-mentioned zinc oxide base nano particle ink by inkjet printing.
The invention has the advantages that：By the present invention in that being used as solvent with alcohol ether ester type compound so that oxidation
Zinc-base nanometer particle ink has suitable boiling point, viscosity, surface tension and the stable zinc oxide base nano that is uniformly dispersed
Grain, wetability after inkjet printing to quantum dot light emitting layer is good, film forming is uniform, solvent is volatile.
Embodiment
Below in conjunction with embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail, shown
So, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other implementation that those of ordinary skill in the art are obtained on the premise of creative work is not made
Mode, belongs to the scope of the present invention.
The present invention provides a kind of zinc oxide base nano particle ink, including solvent and dispersed zinc oxide in a solvent
Base nano particle, by mass percentage, in zinc oxide base nano particle ink of the present invention, zinc oxide base nano particle accounting
0.01-20.00%, solvent accounting 80.00-99.99%, the solvent include at least one alcohol ether ester type compound.Alcohol ether-ether
Class compound contributes to the scattered and infiltration quantum dot light emitting layer of zinc oxide base nano particle.The polarity of alcohol ether ester type compound compared with
Weak, boiling point is relatively low, and volatilization is easy and fast to after inkjet printing.The zinc oxide base nano particle ink that the present invention is obtained has suitable
Viscosity, surface tension and the stabilization that is uniformly dispersed, in inkjet printing, film forming is excellent, can meet inkjet printing requirement.One
It is individual preferred embodiment in, the mass fraction scope that zinc oxide base nano particle accounts for zinc oxide base nano particle ink is
0.10-5.00%.
The alcohol ether ester type compound of the present invention refers to the compound containing at least one ehter bond He at least one ester bond.One
In individual preferred embodiment, alcohol ether ester type compound refers to that occurring esterification by carboxylic acid and alcohol ether obtains.At one preferably
In embodiment, alcohol ether ester type compound of the invention includes at least one hydroxyl, at least one ehter bond and at least one ester bond.
In one preferred embodiment, by mass percentage, in zinc oxide base nano particle ink, alcohol ether esters
Compound accounting 10.00-80.00%, more preferably 20.00-50.00%.
The alcohol ether ester type compound of the present invention is preferably capable the micromolecular compound volatilized completely.In a specific implementation
In mode, alcohol ether ester type compound boiling spread is 50-300 DEG C.In a detailed embodiment, alcohol ether ester type compound
Carbon atom number range is 4-20.Preferably, the one kind of alcohol ether ester type compound in following material：Ethylene glycol monomethyl ether acetic acid
Ester, ethylene glycol ether acetate, glycol propyl ether acetate, ethylene glycol monomethyl ether n Propanoic acid ester, ethylene glycol ethyl ether n Propanoic acid ester, second
Glycol propyl ether n Propanoic acid ester, ethylene glycol monomethyl ether isopropyl acid esters, ethylene glycol ethyl ether isopropyl acid esters, glycol propyl ether isopropyl acid esters, third
Glycol methyl ether acetate, propylene-glycol ethyl ether acetate, propylene glycol propyl ether acetate, propylene glycol monomethyl ether n Propanoic acid ester, propane diols second
Ether n Propanoic acid ester, propylene glycol propyl ether n Propanoic acid ester, propylene glycol monomethyl ether isopropyl acid esters, propylene-glycol ethyl ether isopropyl acid esters, propane diols third
Ether isopropyl acid esters, diethylene glycol dimethyl ether acetate, diethylene glycol ether acetate, dipropylene glycol methyl ether acetate, DPG
Ethyl ether acetate ester, dipropylene glycol propyl ether acetate, dipropylene acetate.
In a preferred embodiment, under the conditions of 25 DEG C, the range of viscosities of zinc oxide base nano particle ink is 1-
40cP, surface tension range is 20-60mN/m.Another preferred embodiment in, under the conditions of 25 DEG C, zinc oxide base nano
The range of viscosities of particle ink is 2-18cP, and surface tension range is 25-45mN/m.
Further, viscosity modifier can also be included in solvent of the present invention, viscosity modifier includes unitary or polynary
Small molecular alcohol compounds, the mass percent scope that small molecular alcohol compounds account for zinc oxide base nano particle ink is
0.01-60.00%.It is preferred that, the boiling spread of small molecular alcohol compounds is 50-300 DEG C.Small molecular alcohol compounds conduct
The advantage of viscosity modifier is：Boiling point is relatively low, be easy to volatilization, while different type small molecule alcohol chemical combination covers larger model
The viscosity number enclosed, it is easy to adjust ink viscosity.In one preferred embodiment, monohydric alcohol includes the total number of carbon atoms and is less than 15
Alcohol, specifically, including methanol, ethanol, propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, amylalcohol, isoamyl
Alcohol, sec-amyl alcohol, secondary isoamyl alcohol, 3- amylalcohols, tert-pentyl alcohol, cyclopentanol, 2-methyl-1-butene alcohol, 2- methyl anyl alcohols, 4- methyl -2- penta
Alcohol, n-hexyl alcohol, 2- hexanols, 2- ethyl butanols, 2- methyl anyl alcohols, 2- methyl -2- amylalcohols, 2- methyl -3- amylalcohols, 3- ethyls -3-
Amylalcohol, n-heptanol, 2- enanthol, 3- enanthol, 2-Ethylhexyl Alcohol, 2 methyl cyclohexanol, n-octyl alcohol, sec-n-octyl alcohol, 3,5,5- trimethyls
Hexanol, nonyl alcohol, 2,6- 2,6-dimethyl-4-heptanols, Decanol, 5- ethyl -2- nonyl alcohols, undecyl alcohol, 5- ethyl -2- nonyl alcohols, lauryl alcohol,
Exxal 12, cyclohexanol, cis- 2 methyl cyclohexanol, cis- 3 methyl cyclohexanol, cis- 4- methyl ring ethanol, 2- butoxy second
At least one of alcohol, phenmethylol, alpha-phenyl ethyl alcohol, bata-phenethyl alcohol, tridecanol.In one preferred embodiment, polyalcohol
The total number of carbon atoms be less than 10, specifically, including ethylene glycol, 1,2-PD, 1,3-PD, 1,2- butanediols, 1,3- fourths
Glycol, 1,4- butanediols, 2,3- butanediols, 1,5- pentanediols, 2- methyl -2,4-PD, 2,2- dimethyl -1,3- the third two
Alcohol, 2- butene-1s, 4- glycol, 2- methyl -2,4- pentanediol, Pinacol, 2- ethyls -1,3- hexylene glycol,
At least one of glycerine, 1,2,4- butantriols, 1,2,6- hexanetriols, pentaerythrite.
It is preferred that, solvent can also include alkoxide compound in the present invention, and alkoxide compound accounts for zinc oxide base nano
The mass percent scope of particle ink is 0.01-60.00%, more preferably in 10.00-40.00%.Alkoxide compound should
It is the material that can be volatilized completely, it is preferred that the boiling spread of alkoxide compound is 50-300 DEG C.In a preferred embodiment party
In formula, the total number of carbon atoms of the alkoxide compound is less than 20 alcohol ester, specifically, including acetic acid glycol ester, propionic acid second
Diol ester, butyric acid glycol ester, valeric acid glycol ester, propylene glycol acetate, propionic acid propylene glycol ester, butyric acid propylene glycol ester, valeric acid
Propylene glycol ester, acetic acid butanediol ester, propionic acid butanediol ester, butyric acid butanediol ester, valeric acid butanediol ester, acetin, diethyl
Acid glyceride, acetic acid binaryglycol ester, propionic acid binaryglycol ester, butyric acid binaryglycol ester, 2,2,4- trimethyl -1,3- pentanediols
At least one of mono isobutyrate.
In a preferred embodiment, solvent further comprises alcohol ethers compound in the present invention, for improving ink
The film forming of water.The mass percent scope that alcohol ethers compound accounts for the zinc oxide base nano particle ink is 0.01-
60.00%, more preferably in 10.00-40.00%.In one preferred embodiment, alcohol ethers compound includes ethylene glycol first
Ether, ethylene glycol ethyl ether, glycol propyl ether, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propylene glycol propyl ether, propane diols fourth
Ether, butanediol methyl ether, butanediol ether, butanediol propyl ether, butanediol butyl ether, diethylene glycol ether, diethylene glycol dimethyl ether, diethyl two
Diethylene glycol dimethyl ether, diethylene glycol ether, diethylene glycol diethyl ether, diethylene glycol propyl ether, diethylene glycol dipropyl ether, diethylene glycol fourth
Ether, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, dipropylene glycol methyl ether, dimethyl ether, DPE, two
At least one of propane diols diethyl ether, dipropylene, tri ethylene glycol ethyl ether, tripropylene glycol methyl ether, tripropylene glycol butyl ether.
In order to reduce the defect of zinc oxide base nano particle surface, and increase zinc oxide base nano particle dispersiveness,
Solvent is preferably also comprising at least one dispersant in the present invention, and dispersant preferably includes alcamine compound or thio-alcohol chemical combination
Thing.Dispersant preferably can include monoethanolamine, diethanol amine, triethanolamine, N methyldiethanol amine, N- ethyldiethanolamines,
N- n-propyls diethanol amine, N- isopropyldiethanolamines, N- n-butyldiethanolamines, normal propyl alcohol amine, isopropanolamine, diisopropanol
At least one of amine, butanolamine, amylalcohol amine, dithioglycol.In small molecular alcohol aminated compounds or sulfur alcohol compound
Nitrogen-atoms or sulphur atom can produce good coordination with the Zn-ef ficiency of zinc oxide base nano particle surface, effectively subtract
Lack its surface defect, add the compatibility of zinc oxide base nano particle and solvent.
The particle diameter of zinc oxide base nano particle can be 1-100nm in the present invention.In order to reduce zinc oxide base nano particle
The defect that dimensional effect is brought, the particle diameter of zinc oxide base nano particle is preferably 2-10nm.
Further, in order to meet the level-density parameter from different emitting layer materials, the present invention can be mixed by metal ion
Miscellaneous or oxide-doped mode changes the band gap of zinc oxide base nano particle.At one preferred embodiment, zinc oxide
Base nano particle includes Zinc oxide nanoparticle, metal ion mixing or oxide-doped Zinc oxide nanoparticle.Specifically,
Zinc oxide base nano particle includes zinc oxide, magnesium zinc oxide, tungsten oxide zinc, titanium oxide zinc, oxidation nickel zinc, zinc tin oxide, oxidation
At least one of tin titanium zinc, magnesium oxide titanium zinc, it should be noted that binary or three-component compound system zinc oxide base nano
The ratio of metallic element can be adjusted according to the actual requirements in grain.In the present invention, zinc oxide base nano particle passes through liquid phase legal system
It is standby.
The present invention also provides a kind of embodiment for preparing as above any described zinc oxide base nano particle ink, and it is wrapped
Include step：It is first according to above-mentioned formula zinc oxide base nano particle is dispersed in alcohol ether ester type compound, then fully vibration
Or stirring, obtain zinc oxide base nano particle ink.
Above-mentioned obtained zinc oxide base nano particle ink is respectively provided with suitable viscosity, surface tension and solvent hair speed
Rate, and the stabilization that is uniformly dispersed, good film-forming property after printing can meet inkjet printing requirement.
The invention also discloses a kind of electroluminescent device, the electron transfer layer of electroluminescent device is zinc oxide base nano
Stratum granulosum, electron transfer layer is prepared by any of the above-described zinc oxide base nano particle ink of inkjet printing.Due to oxygen in the present invention
Change polarity, boiling point, viscosity of solvent of zinc-base nanometer particle ink etc. suitable so that the inkjet printing of ink is smooth, after printing
Solvent it is volatile, prepared electron transfer layer film forming is uniform.
Below with reference to embodiment and comparative example, beneficial effects of the present invention are further illustrated.
Embodiment 1
The zinc oxide base nano particle ink composition that the present embodiment is provided is zinc oxide base nano particle and alcohol ether esters
Compound.Specifically, by mass percentage, including 3.00% Zinc oxide nanoparticle, 60.00% ethylene glycol monomethyl ether acetic acid
Ester and 37.00% dipropylene acetate.
Embodiment 2
The zinc oxide base nano particle ink composition that the present embodiment is provided is zinc oxide base nano particle, alcohol ether esters chemical combination
Thing and small molecule alcohol.Specifically, by mass percentage, including 3.00% magnesium zinc oxide nano particle, 50.00%
Propylene glycol methyl ether acetate and 47.00% Decanol.
Embodiment 3
The zinc oxide base nano particle ink composition that the present embodiment is provided is zinc oxide base nano particle, alcohol ether esters chemical combination
Thing, small molecule alcohol and alkoxide compound.Specifically, by mass percentage, including 3.00% magnesium zinc oxide nanometer
Particle, 50.00% dipropylene acetate, 30.00% 2- methyl -2,4-PD and 17.00% 2,2,4-
Trimethyl -1,3- pentanediol mono isobutyrates.
Embodiment 4
The zinc oxide base nano particle ink composition that the present embodiment is provided is zinc oxide base nano particle, alcohol ether esters chemical combination
Thing, small molecule alcohol, alkoxide compound and alcamine compound.Specifically, by mass percentage, including 3.00%
Magnesium zinc oxide nano particle, 45.00% glycol methyl ether acetate, 20.00% 1,3- propane diols, 25.00% butyric acid
Binaryglycol ester and 7.00% monoethanolamine.
Embodiment 5
The zinc oxide base nano particle ink composition that the present embodiment is provided is zinc oxide base nano particle, alcohol ether esters chemical combination
Thing, small molecule alcohol, alkoxide compound and alcamine compound.Specifically, by mass percentage, including 2.00%
Zinc oxide nanoparticle, 30.00% propylene glycol methyl ether acetate, 30.00% 1,3- propane diols, 30.00% 2,2,4-
Trimethyl -1,3- pentanediol mono isobutyrates and 8.00% monoethanolamine.
Embodiment 6
The present embodiment provides a kind of electroluminescent device, and its preparation method comprises the following steps：The spin coating on ito anode layer
PEDOT：PSS materials, then 120 DEG C of annealing 30min, form hole injection layer；Then TFB materials are formed on hole injection layer
Material, 150 DEG C of annealing 30min, forms hole transmission layer；Spin coating feux rouges CdSe/ is utilized on the hole transmission layer as supporting part
ZnS quantum dot solution formation quantum dot light emitting layer；Zinc oxide nanoparticle ink on luminescent layer in inkjet printing embodiment 5
Water, electron transfer layer is formed after drying；Last evaporating Al negative electrode layer, encapsulation forms electroluminescent device.
In the present embodiment, Zinc oxide nanoparticle ink is good with luminescent layer wetability, after drying, electron transfer layer film forming
It is smooth and uniform.
Comparative example 1
This comparative example provides a kind of electroluminescent device, and its preparation method is same as Example 6, and different is, electricity
Sub- transport layer is prepared by the ethanol solution of spin coating Zinc oxide nanoparticle, wherein, Zinc oxide nanoparticle and institute in embodiment 6
The Zinc oxide nanoparticle used is identical.In this comparative example, the electron transfer layer film forming prepared by spin coating mode is smooth and equal
It is even.
Under the conditions of 25 DEG C, to the viscosity and surface tension of zinc oxide base nano particle ink of the embodiment 1 into embodiment 5
Test result such as following table：
| Embodiment | Viscosity (cp) | Surface tension (mN/m) |
| Embodiment 1 | 2.3 | 30.1 |
| Embodiment 2 | 7.2 | 29.5 |
| Embodiment 3 | 8.0 | 31.2 |
| Embodiment 4 | 5.4 | 29.8 |
| Embodiment 5 | 13.5 | 32.5 |
From test result as can be seen that being adjusted by the content to each component in solvent, range of viscosities can be obtained
Relatively wide, the appropriate zinc oxide base nano particle ink of surface tension, prepared zinc oxide base nano particle ink can be met
Demand of the different ink-jet printers to ink performance.
To embodiment 6 and the test result of the electroluminescent properties of the electroluminescent device of comparative example 1 such as following table：
| High-high brightness (cd/A) | Maximum external quantum efficiency (%) | |
| Embodiment 6 | 15.3 | 11.0 |
| Comparative example 1 | 17.0 | 12.5 |
From test result as can be seen that compared with spin coating mode prepares electron transfer layer, passing through the electricity of inkjet printing mode
The high-high brightness of electroluminescence device and maximum external quantum efficiency are substantially suitable.Due to preparing electron transfer layer by spin coating mode
Technique more ripe, good film-forming property, test result shows that zinc oxide base nano particle ink can not only meet ink-jet in the present invention
The demand to ink performance is printed, meanwhile, electroluminescent device function admirable.
The invention provides a kind of zinc oxide base nano particle ink formula and preparation method thereof, Zinc oxide-base can be made to receive
Rice grain stable and uniform it is scattered in a solvent, and obtain more suitable viscosity and surface tension.By viscosity modifier,
Dispersant etc. so that the viscosity of ink has larger adjustable range, can meet demand of the different ink-jet printers to ink.More
Further, zinc oxide base nano particle ink is preferable with luminescent layer wellability during inkjet printing, realizes high-quality film forming,
Thus avoid the phenomenons such as dry and cracked, orange peel, shrinkage cavity easily occur.Solvent in inkjet printing rear oxidation zinc-base nanometer particle ink holds very much
Easily quick volatilization, noresidue.The performance of prepared electroluminescent device is improved.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in protection scope of the present invention.
Claims (17)
1. a kind of zinc oxide base nano particle ink, including solvent and the zinc oxide base nano being dispersed in the solvent
Grain, by mass percentage, in the zinc oxide base nano particle ink, the zinc oxide base nano particle accounting 0.01-
20.00%, the solvent accounting 80.00-99.99%, it is characterised in that the solvent includes at least one alcohol ether esters chemical combination
Thing.
2. zinc oxide base nano particle ink according to claim 1, it is characterised in that by mass percentage, described
In zinc oxide base nano particle ink, the alcohol ether ester type compound accounting 10.00-80.00%.
3. zinc oxide base nano particle ink according to claim 1, it is characterised in that under the conditions of 25 DEG C, the oxidation
The range of viscosities of zinc-base nanometer particle ink is 1-40cP.
4. zinc oxide base nano particle ink according to claim 1, it is characterised in that under the conditions of 25 DEG C, the oxidation
The surface tension range of zinc-base nanometer particle ink is 20-60mN/m.
5. zinc oxide base nano particle ink according to claim 1, it is characterised in that the alcohol ether ester type compound
Boiling spread is 50-300 DEG C.
6. zinc oxide base nano particle ink according to claim 5, it is characterised in that the alcohol ether ester type compound bag
Include glycol methyl ether acetate, ethylene glycol ether acetate, glycol propyl ether acetate, ethylene glycol monomethyl ether n Propanoic acid ester, second two
Alcohol ether n Propanoic acid ester, glycol propyl ether n Propanoic acid ester, ethylene glycol monomethyl ether isopropyl acid esters, ethylene glycol ethyl ether isopropyl acid esters, second two
Alcohol propyl ether isopropyl acid esters, propylene glycol methyl ether acetate, propylene-glycol ethyl ether acetate, propylene glycol propyl ether acetate, propylene glycol monomethyl ether
N Propanoic acid ester, propylene-glycol ethyl ether n Propanoic acid ester, propylene glycol propyl ether n Propanoic acid ester, propylene glycol monomethyl ether isopropyl acid esters, propylene-glycol ethyl ether
Isopropyl acid esters, propylene glycol propyl ether isopropyl acid esters, diethylene glycol dimethyl ether acetate, diethylene glycol ether acetate, DPG first
At least one in ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropylene acetate
Kind.
7. zinc oxide base nano particle ink according to claim 1, it is characterised in that the solvent is adjusted comprising viscosity
Agent, the viscosity modifier includes unitary or polynary small molecular alcohol compounds of the boiling spread for 50-300 DEG C, described small
The mass percent scope that molecule alcohol compound accounts for the zinc oxide base nano particle ink is 0.01-60.00%.
8. zinc oxide base nano particle ink according to claim 7, it is characterised in that the small molecular alcohol compounds
Including ethanol, propyl alcohol, butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, amylalcohol, isoamyl alcohol, sec-amyl alcohol, secondary isoamyl alcohol, hexanol, heptan
Alcohol, octanol, nonyl alcohol, ten carbon alcohol, undecylenic alcohol, Lauryl Alcohol, 13 carbon alcohol, positive ethylene glycol, 1,2-PD, 1,3- the third two
Alcohol, 1,2- butanediols, 1,3-BDO, BDO, 2,3-butanediol, 1,5-PD, 2- methyl -2,4- pentanediol,
NPG, 2- butene-1s, 4- glycol, 2- methyl -2,4- pentanediol, 2,3- dimethyl -2,3- fourth two
At least one of alcohol, 2- ethyls -1,3- hexylene glycol, glycerine, BT, 1,2,6- hexanetriols, pentaerythrite.
9. zinc oxide base nano particle ink according to claim 1, it is characterised in that the solvent includes boiling spread
For 50-300 DEG C of alkoxide compound, the alkoxide compound accounts for the quality percentage of the zinc oxide base nano particle ink
It is 0.01-60.00% than scope.
10. zinc oxide base nano particle ink according to claim 9, it is characterised in that the alkoxide compound bag
Include acetic acid glycol ester, propionic acid glycol ester, butyric acid glycol ester, valeric acid glycol ester, propylene glycol acetate, propionic acid propane diols
Ester, butyric acid propylene glycol ester, valeric acid propylene glycol ester, acetic acid butanediol ester, propionic acid butanediol ester, butyric acid butanediol ester, valeric acid fourth two
Alcohol ester, acetin, diacetine, acetic acid binaryglycol ester, propionic acid binaryglycol ester, butyric acid binaryglycol ester, 2,
At least one of 2,4- trimethyl -1,3- pentanediol mono isobutyrates.
11. zinc oxide base nano particle ink according to claim 1, it is characterised in that the solvent includes alcohol ethers
Compound, the mass percent scope that the alcohol ethers compound accounts for the zinc oxide base nano particle ink is 0.01-
60.00%.
12. zinc oxide base nano particle ink according to claim 11, it is characterised in that the alcohol ethers compound bag
Include ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol propyl ether, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, propane diols third
Ether, propandiol butyl ether, butanediol methyl ether, butanediol ether, butanediol propyl ether, butanediol butyl ether, diethylene glycol ether, diethylene glycol
Methyl ether, diethylene glycol dimethyl ether, diethylene glycol ether, diethylene glycol diethyl ether, diethylene glycol propyl ether, diethylene glycol dipropyl ether,
Butyl, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, dipropylene glycol methyl ether, dimethyl ether, DPG
In single ether, dipropylene glycol diethyl ether, dipropylene, tri ethylene glycol ethyl ether, tripropylene glycol methyl ether, tripropylene glycol butyl ether
It is at least one.
13. zinc oxide base nano particle ink according to claim 1, it is characterised in that the solvent includes dispersant,
The dispersant includes alcamine compound or sulfur alcohol compound.
14. zinc oxide base nano particle ink according to claim 13, it is characterised in that the dispersant includes ethanol
Amine, diethanol amine, triethanolamine, N methyldiethanol amine, N- ethyldiethanolamines, N- n-propyls diethanol amine, N- isopropyls
Diethanol amine, N- n-butyldiethanolamines, normal propyl alcohol amine, isopropanolamine, diisopropanolamine (DIPA), butanolamine, amylalcohol amine, dithioglycol
At least one of.
15. zinc oxide base nano particle ink according to claim 1, it is characterised in that the zinc oxide base nano
The particle size range of grain is 1-100nm.
16. zinc oxide base nano particle ink according to claim 1, it is characterised in that the zinc oxide base nano
Grain includes Zinc oxide nanoparticle, metal ion mixing or oxide-doped Zinc oxide nanoparticle.
17. a kind of electroluminescent device, including negative electrode, electron transfer layer, luminescent layer, hole transmission layer and anode, its feature exist
In the electron transfer layer any zinc oxide base nano particle ink in claim 1-16 passes through inkjet printing system
It is standby.
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Application publication date: 20170829 |