CN109929330A - Inorganic nano material prints ink and its preparation method and application - Google Patents
Inorganic nano material prints ink and its preparation method and application Download PDFInfo
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- CN109929330A CN109929330A CN201711347576.5A CN201711347576A CN109929330A CN 109929330 A CN109929330 A CN 109929330A CN 201711347576 A CN201711347576 A CN 201711347576A CN 109929330 A CN109929330 A CN 109929330A
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Abstract
The present invention provides a kind of inorganic nano materials to print ink, it is organic solvent that inorganic nano material, which prints the solvent in ink, it includes at least one inorganic nano material and at least one phosphorous acid esters organic solvent that inorganic nano material, which prints ink, the structure of phosphorous acid esters organic solvent for example Formulas I, II, III, IV it is any shown in:Formulas IFormula IIFormula IIIFormula IV wherein, R1、R2、R3Aliphatic group or aromatic group independently selected from H, C1-30, and R1、R2、R3In at most only one be H；R4Aliphatic group or aromatic group selected from C1-30；R5Selected from H, alkyl or alkyl derivative；R6Selected from H, alkyl or alkyl derivative；A, b, c are independently chosen from the integer of 0-3, and a+b+c=3.
Description
Technical field
The invention belongs to electroluminescent diode field of display technology more particularly to a kind of inorganic nano material to print ink
And its preparation method and application.
Background technique
Quantum dot (quantum dot, QD), but can be described as it is nanocrystalline, be it is a kind of by semiconductor material (usually by IIB~
VI A or IIIA~VA element) composition nano particle.Quantum dot is the Nano semiconductor material of zero dimension (zero-dimensional)
Material, the size of three of them dimension are all not more than twice of the exciton Bohr radius of its corresponding semiconductor material, the property of quantum dot
It can generally be influenced by quantum confined effect (quantum confinement effect), skin effect and doping.Quantum dot
Generally spherical or spherical, partial size is stablized between 2~20nm, since electrons and holes are by quantum confinement, continuous energy
Band structure becomes the discrete energy level structure with molecular characterization, and fluorescence can be emitted after being excited.Quantum dot has novel electronics
Ensure that luminescent color can cover the entire visual field from blue light to feux rouges with performances, the chemical components of quantum dot such as optics, and
And excitation purity is high, continuously adjustable, is the material with breakthrough industrial application.In recent years, quantum dot light emitting material shines in LED
The fields such as bright, liquid crystal display have played very big effect, and quantum dot substitutes traditional fluorescent powder, effectively improve LED and
The colour gamut of liquid crystal display.Recently, luminescent material is as the light emitting diode with quantum dots (QLED) of luminescent layer in solid-state lighting, plate
The fields such as display are with a wide range of applications, and receive the extensive concern of academia and industrial circle.
The solution processing properties of quantum dot allow quantum dot light emitting layer to pass through spin coating, blade coating, injection, inkjet printing etc.
Various ways preparation.Opposite front several method, inkjet printing technology can be accurately in the desired amount by quantum dot light emitting material
Deposit it is in place, allow semiconductor material uniform deposition formed film layer.Quantum dot light emitting layer, material are prepared by inkjet printing
The utilization rate of material is very high, and manufacturer can reduce production cost, simplifies manufacture craft, is easy universal volume production, reduces cost.Spray
Black printing technique is the effective ways of the manufacture problem that can solve large scale QLED screen generally acknowledged at present.
However, inkjet printing technology needs to prepare suitable ink, ink needs evenly dispersed and performance to stablize.Firstly,
Ink-jet printing ink needs enough dispersibilities and hydrophobicity, and nanoparticle is uniformly dispersed under solution state.But
Quantum dot ink is essentially all that quantum dot is directly dispersing in solvent at present, the good solvent of relative distribution such as toluene, chlorine
It imitates, obtained quantum dot ink boiling point is lower, and viscosity is also very small；, viscosity biggish solvent higher for some boiling points is such as
Long alkane alcohols solvent, it is again very poor to the dispersion effect of quantum dot.Ink quickly volatilizees the quantum dot picture for often leading to print
Vegetarian refreshments shape is uncontrollable, and the thickness uniformity is very poor, and there are various emission defects, such as Mura (to refer to display brightness for obtained film layer
Unevenly, the phenomenon that causing various traces) unevenness problem, cause uniformity among pixels poor.Quantum dot ink and common ink
Difference, for introducing insulating properties organic material few as far as possible in the quantum dot film layer that finally prints, to keep quantum interlayer charge
Effectively, solute only has quantum dot in general ink for transmission.Secondly, ink-jet printing ink also needs to have viscosity appropriate, surface
Tension.Suitable viscosity and surface tension not only may be implemented printer and stablize ink-jet, it is also possible that ink is in picture element matrix
Interior stabilization is sprawled, and is improved wetability, is effectively prevent excessive and avoid sprawling not in place.Meanwhile suitable viscosity and surface are opened
Power can also realize that solvent is uniformly spread in ink curing processes, prevent from forming the non-uniform ink droplet film such as coffee ring.Therefore,
For quantum dot ink, need to find one kind can viscosity it is adjustable while there is preferable dispersibility, and can post-process
Facilitate the solvent of removal in journey, so that quantum dot ink can satisfy inkjet printing requirement, stablize out of ink, high wettability, stablizes
It sprawls, uniform drying, forms a film uniform.
Summary of the invention
The purpose of the present invention is to provide adjustable inorganic nano material printing ink of a kind of viscosity and preparation method thereof, purports
(viscosity, the surface tension, dispersion of ink are mainly printed solving existing inorganic nano material printing ink comprehensive stability
Property, rate of volatilization) it is difficult to the problem of taking into account.
Inorganic nano is prepared using above-mentioned inorganic nano material printing ink another object of the present invention is to provide a kind of
The method of material film.
For achieving the above object, The technical solution adopted by the invention is as follows:
A kind of inorganic nano material printing ink, it is organic solvent that the inorganic nano material, which prints the solvent in ink,
The inorganic nano material printing ink includes at least one inorganic nano material and at least one phosphorous acid esters organic solvent,
Shown in the structure of the phosphorous acid esters organic solvent such as general structure I, II, III, IV is any:
Formulas I, in II, III, IV, the R1、R2、R3The aromatic series of aliphatic group, C1-30 independently selected from H, C1-30
Group, and R1、R2、R3In at most only one be H；
The R4The aromatic group of aliphatic group, C1-30 selected from C1-30；
The R5Selected from H, halogen, alkyl or alkyl derivative；
The R6Selected from H, halogen, alkyl or alkyl derivative；
A, b, c are independently chosen from the integer of 0-3, and a+b+c=3.
Correspondingly, a kind of preparation method of above-mentioned inorganic nano material printing ink, comprising the following steps:
Inorganic nano material and organic solvent are provided, it is organic molten at least to contain a kind of phosphorous acid esters in the organic solvent
Agent；
Inorganic nano material is dissolved in organic solvent and forms the inorganic nano material printing ink.
And a kind of preparation method of inorganic nano material film, comprising the following steps:
Above-mentioned inorganic nano material printing ink is provided, or prepares inorganic nano material printing ink according to the method described above；
Ink is printed in deposited on supports inorganic nano using inkjet printing, by being dried, obtains inorganic nano material
Expect film.
Inorganic nano material provided by the invention prints ink, using with general structure I, II, III, IV it is any shown in
Phosphorous acid esters organic solvent, phosphite ester are three-fold coordination phosphorus compound, and phosphite ester is the very high phosphatization of a kind of reactivity
Object is closed, it has the response characteristics such as the distinctive nucleophilic of trivalent phosphorous compound, electrophilic, parents and diene compatibility, can play steady
Determine the effect of quantum dot.On this basis, inorganic nano material provided by the invention prints ink, on the one hand, the phosphorous acid
Based organic solvent viscosity is higher, can effectively increase the viscosity of printing ink, improves quality of forming film.Meanwhile the phosphorous
Esters of gallic acid organic solvent thermal stability with higher is conducive to improve inorganic nano material stably dispersing in organic solvent
Property.On the other hand, the phosphorous acid esters organic solvent is a kind of outstanding antioxidant, and quantum dot can be made broken from oxygen
It is bad, to stablize the film performance after off-set oil ink print, and then stablize the device performance containing the film layer.
Inorganic nano material using the phosphorous acid esters organic solvent as organic solvent constituent prints ink, no
Only assign the adjustable viscosity of the inorganic nano material printing ink, good dispersion stabilization.Moreover, containing above-mentioned specific knot
The inorganic nano material printing ink of the phosphorous acid esters organic solvent of structure has suitable rate of volatilization and surface tension, table
For face tension within the scope of 20-80mN/m, viscosity under the conditions of 25-35 DEG C is 0.5-50.0mPa.s, prints inorganic nano material
Brush ink is uniformly dispersed, stable storage, can satisfy requirement of the current ink-jet printer to viscosity and surface tension, realizes inorganic
The inkjet printing mode of layer of nanomaterial, realize in print procedure stablize it is out of ink, stablize sprawl, high wettability, uniform drying, at
Film is uniform, obtains the inorganic nano material luminescent layer with pixel-matrix, high-resolution, electroexcitation.Meanwhile the present invention provides
Inorganic nano material printing ink have volatile performance appropriate, can make printing prepare inorganic nano material layer in
Organic molecule volatilization completely, obtains the film layer without ink organic solvent and fine and close arrangement, so that inorganic nano material be effectively ensured
Charge transmits between material, reduces threshold voltage, improves efficiency.
To sum up, inorganic nano material provided by the invention printing ink have preferable hydrophobic stability and dispersion performance,
Suitable viscosity and surface tension, volatile performance, particularly suitable inkjet printing prepare inorganic nano material layer, are such as beaten by ink-jet
Impression method prepares the inorganic nano material luminescent layer in light emitting diode.
The preparation method of inorganic nano material provided by the invention printing ink, inorganic nano material need to be only dissolved in containing
It is easy to operate easily-controllable in the organic solvent of the phosphorous acid esters solvent of specific structure, do not need harsh condition, it can be achieved that
Produce in enormous quantities.
The preparation method of inorganic nano material film provided by the invention, only need to be by inorganic nano material in organic solvent
It is fully dispersed, inorganic nano material is made and prints ink, and then progress inkjet printing, drying can be obtained on carrier, method
Simply, 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.
The embodiment of the invention provides a kind of inorganic nano materials to print ink, and the inorganic nano material prints in ink
Solvent be organic solvent, inorganic nano material printing ink includes that at least one inorganic nano material and at least one are sub-
Phosphoric acid ester organic solvent, the structure of the phosphorous acid esters organic solvent such as general structure I, II, III, IV are any shown:
Formulas I, in II, III, IV, the R1、R2、R3The aromatic series of aliphatic group, C1-30 independently selected from H, C1-30
Group, and R1、R2、R3In at most only one be H；
The R4The aromatic group of aliphatic group, C1-30 selected from C1-30；
The R5Selected from H, halogen, alkyl or alkyl derivative；
The R6Selected from H, halogen, alkyl or alkyl derivative；
A, b, c are independently chosen from the integer of 0-3, and a+b+c=3.
Inorganic nano material provided in an embodiment of the present invention prints ink, using any with general structure I, II, III, IV
Shown in phosphorous acid esters organic solvent, phosphite ester be three-fold coordination phosphorus compound, phosphite ester is that a kind of reactivity is very high
Phosphorus compound, it has the response characteristics such as the distinctive nucleophilic of trivalent phosphorous compound, electrophilic, parents and diene compatibility, can be with
Play the role of stable quantum dot.On this basis, inorganic nano material provided in an embodiment of the present invention prints ink, a side
Face, the phosphorous acid esters organic solvent viscosity is higher, can effectively increase the viscosity of printing ink, improves quality of forming film.
Meanwhile the phosphorous acid esters organic solvent thermal stability with higher, be conducive to improve inorganic nano material organic molten
Dispersion stabilization in agent.On the other hand, the phosphorous acid esters organic solvent is a kind of outstanding antioxidant, can the amount of making
Son point is destroyed from oxygen, to stablize the film performance after off-set oil ink print, and then stablizes the device performance containing the film layer.
In the embodiment of the present invention, as the R1、R2、R3、R4、R5、R6It, can be with when independently being alkyl or alkyl derivative
For substituted or unsubstituted group.And work as the R1、R2、R3、R4、R5、R6When independently being substituted alkyl or alkyl derivative,
The quantity of substituted mode, substituent group does not limit strictly.Preferably, the R1、R2、R3、R4、R5、R6In independently contain alkane
Base, aryl, nitro, cyano, amino ,-N (R ') (R "), halogen, hydroxyl, carboxyl, ester group, ether, carbonyl, alkenyl, alkynyl, ring
Alkyl, alkoxy, aryloxy group, heteroaryloxy, alkoxy carbonyl group, perfluoroalkyl, perfluoro alkoxy, aryloxy group, thio alkoxy ,-S
(O)2- N (R ') (R ") ,-C (=O)-N (R ') (R "), (R ') (R ") alkyl, (R ') (R ") positive alkoxy, (R ') (R ") nalka
At least one of base aryloxy alkyl ,-S (O) s- aryl or-S (O) s- heteroaryl, silyl-group, wherein the value of s
Range is 0-2.Phosphorous acid esters organic solvent containing above structure, when printing the solvent of ink as inorganic nano material,
Assign inorganic nano material printing ink viscosity appropriate, chemical stability, surface-active.
Further, above-mentioned-N (R ') (R ") ,-S (O)2- N (R ') (R ") ,-C (=O)-N (R ') (R "), (R ') (R ") are just
Alkyl, (R ') (R ") positive alkoxy, in (R ') (R ") alkyl aryloxy group alkyl based structures, the R ', R " are independently selected from substitution
Or unsubstituted alkyl, naphthenic base, aryl.Specific preferred, the alkyl can be straight chained alkyl or branched alkyl, including but
It is not limited to include methyl, ethyl, propyl, isopropyl, isobutyl group, sec-butyl, tert-butyl, amyl, isopentyl, neopentyl, hexyl, different
Hexyl；The naphthenic base includes but is not limited to include cyclopenta, cyclohexyl.The embodiment of the present invention is replaced by alkyl, naphthenic base etc.
Group can be further improved the dissolubility of solvent, convenient for preparing the inorganic nano material factor ink of foam printing.The virtue
Base includes but is not limited to phenyl, xenyl, triphenyl base, benzo base, naphthalene, anthryl, phenalene, phenanthryl, fluorenyl, pyrenyl,
Qu Ji, base, Azulene and heteroaryl compound.Further, the heteroaryl compound includes but is not limited to dibenzo thiophene
Pheno, dibenzofurans, furans, thiophene, benzofuran, benzothiophene, carbazole, pyrazoles, imidazoles, triazole, isoxazole, thiazole,
Oxadiazoles, oxatriazole, dioxazole, thiadiazoles, pyridine, pyridazine, pyrimidine, pyrazine, triazine, oxazines, oxathiazine,
Oxadiazine, indoles, benzimidazole, indazole, indoxazine, benzoxazoles, benzisoxazole, benzothiazole, quinoline
Quinoline, isoquinolin, cinnoline, quinazoline, quinoxaline, naphthalene, phthalein, pteridine, xanthene, acridine, azophenlyene, phenthazine, phenoxazine
Piperazine, dibenzoselenophene, benzoselenophene, benzofuropyridine, indolocarbazole,
Pyridylindole, pyrrolodipyridine, furodipyridine, benzothienopyridine,
Thienodipyridine, benzoselenophenopyridine, selenophenodipyridine.
Specific preferred, the phosphorous acid esters organic solvent is selected from diphenyl iso-octyl phosphite ester, two fourth of phosphorous acid
Ester, bis- (2- ethylhexyl) phosphite esters, three (nonyl phenol) phosphite esters, positive third rouge of phosphite ester two, triisopropyl phosphorous acid
Ester, diisopropyl phosphite, tri iso octyl phosphorite, three (2- chloroethyl) phosphite esters, trimethylolpropane phosphite ester,
Triethyl phosphite, three (2,2,2- trifluoroethyl) phosphite esters, list (trimethylsilyl) phosphite ester, didecyl phosphite,
Didecyl phenyl phosphites, three (3- propylene oxide methanol -3- ethyl) phosphite esters, double dodecyl nonyl phenylphosphonous acids
Ester, one benzene diisodecyl ester of phosphorous acid, phosphorous acid two (dodecyl) rouge, diethyl trimethyl silyl phosphite, acetyl phosphorous
Diethyl phthalate, triethyl phosphite, diethyl phosphite, dibenzyl phosphite, diphenyl phosphite, triphenyl phosphite, Asia
The just own ester of tri-2-ethylhexyl phosphate, phosphorous acid three, phosphorous acid-benzene dioctyl ester, biphenyl phosphorous acid 2- ethylhexyl, three
One of (trimethyl silane) phosphite ester is a variety of.The phosphorous acid esters organic solvent can be in above-mentioned solvent
One kind can also be combined using a variety of in above-mentioned solvent, form mixed solvent.Preferred phosphorous acid esters organic solvent
Type viscosity with higher, preferable stably dispersing performance and appropriate surface tension, and can be in the post-processing after film forming
It is completely removed by modes such as heating, cooling, decompressions, will not influence the inorganic nano material film layer that inkjet printing is prepared,
Particularly suitable inkjet printing prepares inorganic nano material layer, such as quantum dot light emitting layer.
In the embodiment of the present invention, the needs based on inkjet printing, solvent temperature is too high or too low all to be unfavorable for forming densification
The film layer of arrangement.Specifically, printing ink during inkjet printing prepares film layer, wave by solvent when solvent boiling point is too low
Hair is unable to satisfy inkjet printing requirement to influence the overall performance (such as dispersion performance, viscosity, surface tension) of printing ink；
It when solvent boiling point is excessively high, need to could remove, will affect in this way molten in printing ink by high temperature in subsequent film forming procedure
The performance of matter ingredient such as inorganic nano material, such as causes the fluorescent quenching of quantum dot.Specifically, in the embodiment of the present invention, it is described
The boiling point of phosphorous acid esters organic solvent is 130 DEG C -350 DEG C.Above-mentioned phosphorous acid esters provided in an embodiment of the present invention are organic molten
Agent has suitable boiling point, and inkjet printing prepares suitable volatile performance when inorganic nano material layer, can be from dicyandiamide solution
Evaporation is completed, to form the film layer of fine and close arrangement.
In the embodiment of the present invention, the phosphorous acid esters organic solvent for meeting above-mentioned specific structure has suitable viscosity
And surface tension.Specifically, range of viscosities of the phosphorous acid esters organic solvent at 25 DEG C is 0.5mPa.s-50mPa.s,
Surface tension at 25 DEG C is 20-80mN/m.Above-mentioned phosphorous acid esters solvent provided in an embodiment of the present invention all has conjunction
Suitable viscosity and surface tension can satisfy requirement of the current ink-jet printer to viscosity and surface tension, realize inorganic nano
The inkjet printing mode of material layer obtains the inorganic nano material luminescent layer with pixel-matrix, high-resolution, electroexcitation.
In the embodiment of the present invention, the organic solvent of the inorganic nano material printing ink can contain only above-mentioned phosphorous
One of esters of gallic acid organic solvent type, or two kinds in above-mentioned phosphorous acid esters organic solvent or class more than two
The combination solvent that type is formed, can also be at least one of above-mentioned phosphorous acid esters organic solvent type and other organic solvents
The mixed solvent of formation, to adjust the inorganic nano material printing volatile performance of ink, dispersion performance, viscosity and surface tension
Balance.
In the embodiment of the present invention, organic and/or inorganic materials, the inorganic nano material are contained in the inorganic nano material ink
It can use one or more.
Specifically, matrix component of the inorganic nano material as inorganic nano material printing ink, can be
IV race, II-VI group, II-V race, iii-v, III-VI race, group IV-VI, I-III-VI race, II-IV-VI race, II-IV-V race
At least one of binary or polynary semiconducting compound.Specifically, the inorganic nano material can be selected from but not limited to
At least one of CdSe, CdS, CdTe, ZnO, ZnSe, ZnS, ZnTe, HgS, HgSe, HgTe, CdZnSe；Be also selected from but
Be not limited to InAs, InP, InN, GaN, InSb, InAsP, InGaAs, GaAs, GaP, GaSb, AlP, AlN, AlAs, AlSb,
At least one of CdSeTe, ZnCdSe.In addition, the inorganic nano material can also be perovskite nanometer particle material, it is special
Not preferably do not shine perovskite nanoparticle, metal nano particle material, metal oxide nanoparticles material and combinations thereof.
The composition form of the inorganic nano material is unrestricted, can be doped or non-doped inorganic nano material,
Wherein, doping refers to that other doped chemicals are also contained in the inside of the inorganic nano material.Specifically, the inorganic nano material
Material can be quanta point material.Wherein, the ligand of the quantum dot include sour ligand, mercaptan ligand, amine ligand, (oxygen) Phosphine ligands,
At least one of phosphatide, soft phosphatide, polyvinylpyridine etc..As specific embodiment, the acid ligand is ten acid, hendecene
At least one of acid, tetradecylic acid, oleic acid, stearic acid；The mercaptan ligand is eight alkyl hydrosulfides, lauryl mercaptan, 18
At least one of alkyl hydrosulfide；The amine ligand includes at least one of oleyl amine, octadecylamine, eight amine；(oxygen) phosphine is matched
Body is at least one of tri octyl phosphine, trioctylphosphine oxide (TOPO).
In the embodiment of the present invention, the structure type of the quantum dot is unrestricted, and it is mixed that uniform mixed type, gradient can be used
Close type, core-shell structure copolymer type or union type.
The printing of inorganic nano material described in the embodiment of the present invention is suitable for inkjet printing quantum dot light emitting layer, when described inorganic
When water content is higher in nano material printing ink, since shipwreck is in volatilization or removal, it is easy residual in the quantum dot ink
It stays, and then influences the performance of the quantum dot light emitting layer formed.In view of this, quantum dot described in the embodiment of the present invention is preferably
Oil-soluble quantum dot.
As particular preferred embodiment, the average-size of the quantum dot is 1-20nm.
Preferably, in the embodiment of the present invention, the total weight by inorganic nano material printing ink is packet in terms of 100%
Include the following component of following weight percentage:
Inorganic nano material 0.01-20.0%；
Organic solvent 0.01-99.9%；
The mass ratio of the i.e. described inorganic nano material and the organic solvent is 0.01-20.0:80-99.9；
Wherein, the phosphorous acid esters organic solvent is contained in the organic solvent, and the phosphorous acid esters are organic molten
Agent accounts for the 1-90% of the organic solvent gross weight.It should be appreciated that in the organic solvent, in addition to the phosphorous acid esters are organic molten
Agent can also contain other organic solvents.
Specifically, above-mentioned phosphorous acid esters organic solvent account for the organic solvent gross weight weight percentage can for 1%,
5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%.It should be appreciated that the inorganic nano material print
In brush ink, the content of the phosphorous acid esters organic solvent is higher, and the performance that corresponding phosphorous acid esters organic solvent plays is got over
Good, the comprehensive performance of the inorganic nano material printing ink is higher (as described in making the organic solvent containing phosphorous acid esters
Volatile performance, the dispersion stabilization that inorganic nano material prints ink are more preferable, and viscosity and surface tension are more suitable), more it is able to satisfy
Inkjet printing requirement.
Gross weight by inorganic nano material printing ink is the weight percent of the inorganic nano material in terms of 100%
Content is 0.1-20.0%, as specific embodiment, the dosage of the inorganic nano material can for 0.1%, 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% etc. is specific
Numerical value content.Further, as a preferred embodiment, the dosage of the inorganic nano material is 4-15%.As a kind of preferred
Mode, the inorganic nano material printing ink are made of the inorganic nano material and the organic solvent, by weight,
The mass ratio of the inorganic nano material and the organic solvent is 4-15:85-96, and the phosphorous acid esters organic solvent accounts for
The 1-50% of the organic solvent gross weight.In addition to the inorganic nano material and institute in the i.e. described inorganic nano material printing ink
It states outside organic solvent, does not contain other auxiliary reagents.
As another preferred embodiment, the mass ratio of the inorganic nano material and organic solvent is 4-15:85-96, and
The phosphorous acid esters organic solvent accounts for the 1-50% of the organic solvent gross weight.Further, described in the embodiment of the present invention
Inorganic nano material, which prints ink, to include auxiliary reagent, and the auxiliary reagent includes but is not limited to: charge transfer agent glues
Spend regulator and dispersing agent.
Wherein, inorganic nano material can be prepared in inorganic nano material printing ink by the charge conveyer
After the bed of material such as quantum dot light emitting layer, charge transport properties are improved, so that charge transmission is more smooth effectively, reduce threshold voltage,
So that electronics, hole may be coextruded radioluminescence.Specific preferred, the charge transfer agent can be polycarbazole, gather
Fluorenes, polyaniline gather to styrene support (to phenylacetylene), polyacetylene, gather to benzene, polythiophene, polypyridine, polypyrrole and its derivative
At least one of or in which at least two formed copolymers or blend, but not limited to this.
When to make the quantum dot ink carry out inkjet printing, ink is suitably discharged from the nozzle of inkjet print head without sending out
Raw blocking, while there is preferable film forming characteristics, it can be printed in ink in the inorganic nano material and viscosity modifier is added.
The viscosity modifier be preferably polyhydroxy-alcohol, alkyl glycol ether or trimethylolpropane, trimethylolethane, casein,
At least one of carboxymethyl cellulose.Specifically, the polyhydroxy-alcohol is ethylene glycol, diethylene glycol (DEG), diethylene glycol, three second two
Alcohol, propylene glycol, dipropylene glycol, hexylene glycol, 1,3 butylene glycol, 1,4- butanediol, 1,5- pentanediol, 2- butylene-1,4-diol and
At least one of 2- methyl -2- pentanediol, 1,2,6- hexanetriol, glycerine, polyethylene glycol and dipropylene glycol, polyvinyl alcohol.Institute
Stating alkyl glycol ether is in polyethylene glycol monobutyl ether, diethylene glycol monoethyl ether, dipropylene glycol monomethyl ether and Propylene glycol n-propyl ether
At least one.
The dispersing agent can effectively be such that the quantum dot is dispersed in the solvent and protect the dispersion
It is fixed to keep steady.Specifically, the dispersing agent can be one or more surfactants.The surfactant can be anion
Type, cationic, non-ionic or amphoteric surfactant.
As specific embodiment, the nonionic surfactant includes but is not limited to straight chain or second level alcohol ethoxylates
Object, phosphorous acid esters surfactant, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, gathers at alkyl phenol polyoxyethylene ether
Ethylene oxide block copolymer and propoxylated block copolymers, polyoxyethylene and propyl silica resin based surfactants, alkane
At least one of alkyl polyglucosides and acetylenic polyethylene oxides surfactant.The anionic surfactant include but
It is not limited to carboxylate (for example, ether carboxylate and sulfosuccinate), sulfate (for example, lauryl sodium sulfate), sulfonate
(for example, dodecyl benzene sulfonate, α olefin sulfonate, p alkylphenylaceticacid, fatty acid taurides, alkylnaphthalene
Sulfonate), phosphate (for example, alkyl and aryl alcohol phosphate), phosphonate and amine oxide surfactant and anion fluorine
Change at least one of surfactant.The amphoteric surfactant includes but is not limited to trimethylamine second lactones, sulfobetaines
At least one of alkali and alanine rouge.The cationic surfactant include but is not limited to quaternary ammonium compound, sun from
At least one of sub- amine oxide, ethoxy fatty amine and imidazoline surfactant.
In order to sufficiently realize in the inorganic nano material printing ink, inorganic nano material prints fully dispersed, can
Other organic solvents are added in inorganic nano material printing ink.Preferably, the weight of other organic solvents
Account for 50% or more of the organic solvent total weight.
Further, other organic solvents are chlorobenzene, o-dichlorohenzene, tetrahydrofuran, methyl phenyl ethers anisole, morpholine, toluene, neighbour
Dimethylbenzene, meta-xylene, paraxylene, n-hexane, methylene chloride, chloroform, 1,4- dioxane, 1,2 2 chloroethenes
Alkane, 1,1,1- trichloroethanes, 1,1,2,2- tetrachloroethanes, naphthane, naphthalane, phenoxytoluene, dodecane, 1- methoxynaphthalene,
1- dibutyl naphthalene, o-dimethoxybenzene, 1- methyl naphthalene, 1,2- dimethylnaphthalene, cyclohexyl benzene, 1,2,4- trimethoxy-benzene, benzene hexane,
In the tetradecane, 1,2- dimethylnaphthalene, 4- isopropyl biphenyl, 2- isopropyl naphthalene, 1-ethylnaphthalene and 1,2,3,4-tetralin extremely
Few one kind.
As a kind of specific preferred embodiment, inorganic nano material printing ink is by the inorganic nano material, described
Organic solvent and auxiliary reagent composition.
The viscosity of inorganic nano material printing ink provided in an embodiment of the present invention, by described organic containing phosphorous acid esters
The dosage and concrete type of solvent are regulated and controled.Inorganic nano material provided in an embodiment of the present invention prints ink, at 25-35 DEG C
Under the conditions of viscosity be 0.5-50.0mPa.s, concretely 1mPa.s, 5mPa.s, 10mPa.s, 15mPa.s, 20mPa.s,
25mPa.s,30mPa.s,35mPa.s,40mPa.s,45mPa.s,50mPa.s；Further, the viscosity of the quantum dot ink
Preferably 25 DEG C of viscosity is preferably 1-30.0mPa.s, and more preferably viscosity under the conditions of 25-35 DEG C is 1-15.0mPa.s.
The surface tension of the inorganic nano material printing ink is 20.0-80.0mN/m, to can flow in ink jet printing process
It freely is discharged from printing head, and there is preferable film forming characteristics.Specifically, stating the surface of inorganic nano material printing ink
Power can be 20.0mN/m, 30.0mN/m, 40.0mN/m, 50.0mN/m, 60.0mN/m, 70.0mN/m, 80.0mN/m.
The phosphorous acid esters organic solvent provided in an embodiment of the present invention has as inorganic nano material printing ink
Solvent component not only assigns the adjustable viscosity of the inorganic nano material printing ink, good dispersion stabilization.Moreover,
The inorganic nano material printing ink of phosphorous acid esters organic solvent containing above-mentioned specific structure has suitable rate of volatilization
And surface tension, for surface tension within the scope of 20-80mN/m, viscosity under the conditions of 25-35 DEG C is 0.5-50.0mPa.s,
So that inorganic nano material printing ink is uniformly dispersed, stable storage, can satisfy current ink-jet printer to viscosity and surface
The inkjet printing mode of inorganic nano material layer is realized in the requirement of power, realizes that stablizing out of ink, stabilization sprawls, is high in print procedure
Wetability, uniform drying, film forming are uniform, obtain that there is the inorganic nano material of pixel-matrix, high-resolution, electroexcitation to shine
Layer.Meanwhile inorganic nano material printing ink provided by the invention has volatile performance appropriate, and printing can be made to prepare
Organic molecule volatilization in inorganic nano material layer completely, obtains the film layer without ink organic solvent and fine and close arrangement, thus
Charge transmits between inorganic nano material is effectively ensured, and reduces threshold voltage, improves efficiency.
Inorganic nano material provided in an embodiment of the present invention prints ink, can be prepared by following methods.
Correspondingly, the embodiment of the invention provides a kind of preparation method of inorganic nano material printing ink, including it is following
Step:
S01., inorganic nano material and organic solvent are provided, at least had containing a kind of phosphorous acid esters in the organic solvent
Solvent；
S02. inorganic nano material is dissolved in organic solvent and forms the inorganic nano material printing ink.
The preparation method of inorganic nano material printing ink provided in an embodiment of the present invention, only need to be molten by inorganic nano material
It is easy to operate easily-controllable in the organic solvent of the phosphorous acid esters solvent containing specific structure, harsh condition is not needed,
It can be achieved to produce in enormous quantities.
Specifically, the type of the phosphorous acid esters organic solvent can be found in above in above-mentioned steps S01, specifically, institute
It states in organic solvent at least containing a kind of organic solvent containing phosphorous acid esters, of course it is to be understood that the organic solvent can be with
Containing other non-phosphorous acid esters organic solvents, and the phosphorous acid esters organic solvent can also contain two in above-mentioned solvent
Kind is two or more.
The inorganic nano material prints the formula of ink and its preferred ingredient, content have hereinbefore been stated, in order to
Length is saved, details are not described herein again.The embodiment of the present invention controls the inorganic nano material by solvent selection and prints ink
Boiling point is at 350 DEG C or less.
In above-mentioned steps S02, inorganic nano material is dissolved in organic solvent, discrete form is unrestricted, can be used and stirs
The mode of mixing is realized.
And the embodiment of the invention also provides a kind of preparation methods of inorganic nano material film, comprising the following steps:
E01., above-mentioned inorganic nano material printing ink is provided, or prepares inorganic nano material off-set oil according to the method described above
Ink；
E02. ink is printed in deposited on supports inorganic nano using inkjet printing, by being dried, obtains inorganic receive
Rice material film.
The preparation method of inorganic nano material film provided in an embodiment of the present invention, only need to be by inorganic nano material organic
It is fully dispersed in solvent, inorganic nano material is made and prints ink, and then progress inkjet printing, drying can obtain on carrier
, method is simple, it is easy to accomplish standardization control.
The method that above-mentioned steps E01 prepares inorganic nano material printing ink is as described above, in order to save length, herein
It repeats no more.
In above-mentioned steps E02, by selecting suitable ink-jet printer to carry out inkjet printing, receive deposited on supports is inorganic
Then solvent flashing is dried to inorganic nano printing ink in rice printing ink.Specifically, the inkjet printing
It is preferred that being realized using piezoelectric ink jet printing or thermal inkjet-printing.It is described to be dried as heating drying, cooling and drying, be dried under reduced pressure
At least one of.As an implementation, individually using heating drying, cooling and drying, one of be dried under reduced pressure progress
It is dried.As another embodiment, dry using heating and be dried under reduced pressure or cooling and drying and being dried under reduced pressure is done
Dry processing.Preferably, the dry temperature of the heating is 30-180 DEG C, time 0-30min；Preferably, the cooling processing
Temperature be 0-20 DEG C；Preferably, the vacuum degree of the reduced pressure treatment is 1 × 10-6Torr is to normal pressure.
It is dried to obtain inorganic nano material film, such as quantum dot film.It is suitable to be dried mode, it can be efficient
Under the premise of removing the organic solvent containing phosphorous acid esters, guarantee the inorganic nano material such as quanta point material not by broken
It is bad.
The inorganic nano material film dry film formed through inkjet printing, thickness is preferably 10-100nm；Further, through spraying
The inorganic nano material film thickness of dry film that ink printing is formed is 20-50nm.
It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of inorganic nano material prints ink, including the stable quantum dot of oleyl amine, organic solvent and auxiliary reagent,
In, the mass ratio of the stable quantum dot of the oleyl amine and organic solvent is 13:87；The organic solvent is by weight percent
The 1- chloronaphthalene and dibutyl phosphite of 75:12 forms, and 1- chloronaphthalene solvent and dibutyl phosphite silicon are refined through water removal, deoxygenation
It is greater than 99.9% to purity；The auxiliary reagent is polypyrrole.
A kind of preparation method of inorganic nano material film, comprising the following steps:
S11. each component is weighed according to the formula of above-mentioned inorganic nano material printing ink；
S12., 500mL single-necked flask is provided, in the case of stirring, the stable red CdSe/ZnS quantum of addition oleyl amine
Point, 1- chloronaphthalene, polypyrrole and dibutyl phosphite, are stirred 30min, obtain quantum dot printing ink composition；
S13. the quantum dot printing ink composition is injected into printing ink-jet printer cartridge, by ink-jet printer in carrier
Upper inkjet printing is printed as 20 × 30um, the red quantum dot layer of 200 × 200ppi of resolution ratio.130 are heated on hot plate
DEG C, nitrogen flow vacuum 1 × 10-6Volatile dry 30min under Torr obtains monochromatic quantum dot luminescent layer.
Embodiment 2
A kind of inorganic nano material printing ink, including the quantum dot and organic solvent that oleyl amine is stable, wherein the oleyl amine
The mass ratio of stable quantum dot and organic solvent is 10:90；The neighbour that the organic solvent is 20:30:40 by weight percent
Dibromobenzene, tetrahydronaphthalene and phosphorous acid-benzene dioctyl ester composition, and o-dibromobenzene, tetrahydronaphthalene and phosphorous acid-benzene dioctyl ester pass through
Water removal, deoxygenation are refined to purity greater than 99.9%.
A kind of preparation method of inorganic nano material film, comprising the following steps:
S21. each component is weighed according to the formula of above-mentioned inorganic nano material printing ink；
S22., 500mL high-density polyethylene bottle is provided, in the case of stirring, successively adds the stable green of oleyl amine
CdZnSe/CdZnS, o-dibromobenzene, tetrahydronaphthalene and phosphorous acid-benzene dioctyl ester, are stirred 30min, obtain quantum dot ink
Composition；
S23. by the quantum dot printing ink composition by ink-jet printer inkjet printing on carrier, it is printed as 20 ×
The green quantum dot layer of 30um, 200 × 200ppi of resolution ratio.150 DEG C, vacuum 1 × 10 are heated on hot plate-5Torr volatilization is dry
Dry 30min obtains monochromatic quantum dot luminescent layer.
Embodiment 3
A kind of inorganic nano material printing ink, the weight percentage with inorganic nano material printing ink are
100% meter, each component comprising following weight percentage:
The stable quantum dot 10% of oleyl amine；
Organic solvent 90%；
Wherein, the stable quantum dot of the oleyl amine blue CdS/CdZnS stable for oleyl amine, (green CdZnSe/CdZnS,
Red CdSe/ZnS quantum dot)；Tridecane, 1-ethylnaphthalene and the phosphorous that the organic solvent is 30:30:30 by weight percent
The just own ester composition of acid three, and dodecane, tetrahydronaphthalene and dimethyl sulfenimide are refined to purity and are greater than through water removal, deoxygenation
99.9%.
A kind of preparation method of inorganic nano material film, comprising the following steps:
S31. each component is weighed according to the formula of above-mentioned inorganic nano material printing ink；
S32., 500mL high-density polyethylene bottle is provided, in the case of stirring, successively adds tridecane, 1-ethylnaphthalene, oil
Amine stabilized blue CdS/CdZnS, (green CdZnSe/CdZnS, red CdSe/ZnS quantum dot) and the just own ester of phosphorous acid three,
It is stirred 30min, obtains quantum dot printing ink composition；
S33. by the quantum dot printing ink composition by ink-jet printer inkjet printing on carrier, it is printed as 20 ×
Blue, green, the red side-by-side quantum dot layer of 30um, 200 × 200ppi of resolution ratio.130 DEG C, 1 are heated on hot plate
×10-6Volatile dry 30min under Torr obtains three primary colours quantum dot light emitting layer.
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 inorganic nano material prints ink, which is characterized in that the solvent in the inorganic nano material printing ink is
Organic solvent, the inorganic nano material printing ink include at least one inorganic nano material and at least one phosphorous acid esters
Organic solvent, the structure of the phosphorous acid esters organic solvent such as general structure I, II, III, IV are any shown:
Formulas I, in II, III, IV, the R1、R2、R3The aromatic series base of aliphatic group, C1-30 independently selected from H, C1-30
Group, and R1、R2、R3In at most only one be H；
The R4The aromatic group of aliphatic group, C1-30 selected from C1-30；
The R5Selected from H, halogen, alkyl or alkyl derivative；
The R6Selected from H, halogen, alkyl or alkyl derivative；
A, b, c are independently chosen from the integer of 0-3, and a+b+c=3.
2. inorganic nano material as described in claim 1 prints ink, which is characterized in that the R1、R2、R3、R4、R5、R6In
Independently containing alkyl, aryl, nitro, cyano, amino ,-N (R ') (R "), halogen, hydroxyl, carboxyl, ester group, ether, carbonyl,
Alkenyl, alkynyl, naphthenic base, alkoxy, aryloxy group, heteroaryloxy, alkoxy carbonyl group, perfluoroalkyl, perfluoro alkoxy, aryloxy group,
Thio alkoxy ,-S (O)2- N (R ') (R ") ,-C (=O)-N (R ') (R "), (R ') (R ") alkyl, (R ') (R ") positive alcoxyl
Base, (R ') (R ") alkyl aryloxy alkyl ,-S (O)sAryl or-S (O)sHeteroaryl, silyl-group, wherein described
R ', R " are 0-2 independently selected from substituted or unsubstituted alkyl, naphthenic base, aryl, the value range of s.
3. inorganic nano material as described in claim 1 prints ink, which is characterized in that the phosphorous acid esters organic solvent
Selected from diphenyl iso-octyl phosphite ester, dibutyl phosphite, bis- (2- ethylhexyl) phosphite esters, three (nonyl phenol) phosphorous acid
Ester, positive third rouge of phosphite ester two, tri isopropyl phosphorite, diisopropyl phosphite, tri iso octyl phosphorite, three (2- chlorine
Ethyl) phosphite ester, trimethylolpropane phosphite ester, triethyl phosphite, three (2,2,2- trifluoroethyl) phosphite esters, list
(trimethylsilyl) phosphite ester, didecyl phosphite, didecyl phenyl phosphites, three (3- propylene oxide methanol -3- second
Base) phosphite ester, double dodecyl nonylphenylphosphites, one benzene diisodecyl ester of phosphorous acid, phosphorous acid two (dodecyl)
Rouge, diethyl trimethyl silyl phosphite, acetyl diethyl phosphite, triethyl phosphite, diethyl phosphite, phosphorous acid
Dibenzyl ester, diphenyl phosphite, triphenyl phosphite, phosphorous acid three (2- ethylhexyl) ester, the just own ester of phosphorous acid three, phosphorous
One of acid-benzene dioctyl ester, biphenyl phosphorous acid 2- ethylhexyl, three (trimethyl silane) phosphite esters are a variety of.
4. inorganic nano material as described in any one of claims 1-3 prints ink, which is characterized in that by weight, institute
The mass ratio for stating inorganic nano material and the organic solvent is 0.01-20.0:80-99.9, and the phosphorous acid esters are organic
Solvent accounts for the 1-90% of the organic solvent gross weight.
5. inorganic nano material as claimed in claim 4 prints ink, which is characterized in that by weight, described inorganic to receive
The mass ratio of rice material and organic solvent is 4-15:85-96, and to account for the organic solvent total for the phosphorous acid esters organic solvent
The 1-50% of weight.
6. inorganic nano material as claimed in claim 5 prints ink, which is characterized in that the inorganic nano material off-set oil
Ink is made of the inorganic nano material and the organic solvent, by weight, the inorganic nano material with it is described organic
The mass ratio of solvent is 4-15:85-96, and the phosphorous acid esters organic solvent accounts for the 1-50% of the organic solvent gross weight.
7. inorganic nano material as claimed in claim 5 prints ink, which is characterized in that the inorganic nano material printing
Ink further includes auxiliary reagent, and the auxiliary reagent is selected from one of charge transfer agent, viscosity modifier and dispersing agent or several
Kind.
8. inorganic nano material as claimed in claim 7 prints ink, which is characterized in that the inorganic nano material off-set oil
Ink is made of the inorganic nano material, the organic solvent and the auxiliary reagent.
9. inorganic nano material as described in any one of claims 1-3 prints ink, which is characterized in that the phosphorous acid esters
The boiling point of organic solvent is 130 DEG C -350 DEG C.
10. inorganic nano material as described in any one of claims 1-3 prints ink, which is characterized in that the phosphite ester
Range of viscosities of the class organic solvent at 25 DEG C is 0.5mPa.s-50mPa.s, and the surface tension at 25 DEG C is 20-80mN/m.
11. a kind of preparation method of the printing of the inorganic nano material as described in claim any one of 1-10 ink, including following step
It is rapid:
Inorganic nano material and organic solvent are provided, at least contain a kind of phosphorous acid esters organic solvent in the organic solvent；
Inorganic nano material is dissolved in organic solvent and forms the inorganic nano material printing ink.
12. a kind of preparation method of inorganic nano material film, comprising the following steps:
Any one of claim 1-10 inorganic nano material is provided and prints ink, or according to claim 12 the method system
Standby inorganic nano material prints ink；
Ink is printed in deposited on supports inorganic nano using inkjet printing, by being dried, it is thin to obtain inorganic nano material
Film.
13. the preparation method of inorganic nano material film as claimed in claim 12, which is characterized in that the drying process
Mode includes heating drying, cooling and drying, at least one of is dried under reduced pressure.
14. the preparation method of inorganic nano material film as claimed in claim 13, which is characterized in that the heating drying
Temperature is 60-180 DEG C, time 0-30min；
The temperature of the cooling and drying is 0-20 DEG C；
The vacuum degree of the drying process is 1 × 10-6Torr is to normal pressure.
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