CN108624137A - Aqueous quantum dot ink - Google Patents
Aqueous quantum dot ink Download PDFInfo
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- CN108624137A CN108624137A CN201710176903.9A CN201710176903A CN108624137A CN 108624137 A CN108624137 A CN 108624137A CN 201710176903 A CN201710176903 A CN 201710176903A CN 108624137 A CN108624137 A CN 108624137A
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- alcohol
- quantum dot
- organic solvent
- dot ink
- aqueous
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- C—CHEMISTRY; METALLURGY
- 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
Abstract
The present invention provides a kind of aqueous quantum dot ink, it is made of quanta point material and at least one alcohol organic solvent, the boiling point of alcohol organic solvent is 120 DEG C 280 DEG C, the general structure of alcohol organic solvent is R (OH) x, wherein, R is substituted or unsubstituted alkyl or cycloalkyl, and x is positive integer.The aqueous quantum dot ink of the present invention can be to avoid the introducing of additive containing only quanta point material and alcohol organic solvent, the influence to obtained quantum dot film charge transport ability.And due to selecting the alcohol organic solvent of higher, it volatilizees at room temperature relatively slow, can effectively avoid the spray nozzle clogging caused by solvent volatilizees when room temperature prints；But the alcohol organic solvent can fully be removed by heating or vacuum drying method after inkjet printing, and the residual of alcohol organic solvent is avoided to impact the film performance being prepared.In addition, the aqueous quantum dot ink of the present invention, the parameters such as viscosity, surface tension also are adapted for inkjet printing requirement.
Description
Technical field
The invention belongs to electroluminescent diode display technology field more particularly to a kind of aqueous quantum dot ink.
Background technology
Semiconductor-quantum-point shines, and high with photochromic purity, luminous quantum efficiency is high, luminescent color is adjustable, service life is long
Equal good characteristics, these features make the light emitting diode with quantum dots (QLED) using quanta point material as luminescent layer be shone in solid-state
The fields such as bright, FPD show preferable application prospect, receive the extensive concern of academia and industrial circle.
Quantum dot, which is dispersed among in solvent, is configured to quantum dot ink, is suitable for solwution method and prepares.At the solution of quantum dot
Reason characteristic allows quantum dot light emitting layer to be prepared by various ways such as spin coating, blade coating, injection, inkjet printing, bat printings.According to
The difference of quantum dot ligand, quantum dot can be divided into oil-soluble quantum dot and water-soluble quantum dot.Inkjet printing (Ink-jet
Printing) technology is widely studied and is applied in opto-electronic device manufacturing field in recent years, especially aobvious as tablet
Show that device, such as Organic Light Emitting Diode (OLED) and QLED are shown in manufacturing technology, it is considered to be solve high cost and realization
The effective way of large area.Inkjet printing technology in combination with based on solution functional material and advanced ink jet printing device come
OLED or QLED display screens are made, the utilization rate and production efficiency of material can be improved, reduce manufacturing cost, improve production capacity.In order to
Guarantee finally obtains high-purity, high performance solute material film after printing to opto-electronic device, is used for the electricity of opto-electronic device
Sub- ink not only requires high-purity, but also the solvent needs for preparing ink are easily removed.Therefore, electric ink is matched
It should avoid that multi-component solvent or introducing was used to be difficult to the additive removed as possible during system.In addition, ink jet printing device
Itself there are higher requirement, such as suitable boiling point, viscosity, surface tension and the solute dispersed evenly and stably to ink
Deng this also brings bigger difficulty to ink formulation.
Currently, having company reports the quantum dot ink for printing.It includes nanoparticle to be reported a kind of if any company
The method of the printable ink formulations of son is obtained by selecting suitable ink solvent, such as toluene and dodecanol
Printable nanoparticle inks and the corresponding film for including nano-particle.There is company to report a kind of for inkjet printing
Quantum dot ink, this ink is comprising certain density quanta point material, organic solvent and has highly viscous alcohols polymer
Additive.Also company discloses a kind of quantum dot ink formulations including material of main part, quanta point material and additive.At this
In a little published patents, in order to regulate and control the physical parameter of ink, these quantum dot inks all include other additives, such as
Alcohols polymer.And the polymeric additive with insulating property (properties) is not easy to remove, and the introducing of this kind of polymer, often reduce
The charge transport ability of quantum dot film has negative effect to the photoelectric properties of photoelectric device, limits it in photoelectric field
Application.
Invention content
The purpose of the present invention is to provide a kind of aqueous quantum dots, it is intended to solve in existing quantum dot ink containing addition
Agent, the problem of influencing the charge transport ability of quantum dot film.
The invention is realized in this way a kind of aqueous quantum dot ink, organic by quanta point material and at least one alcohols
Solvent forms, and the boiling point of the alcohol organic solvent is 120 DEG C -280 DEG C, and the general structure of the alcohol organic solvent is R-
(OH)x, wherein the R is substituted or unsubstituted alkyl or cycloalkyl, and the x is positive integer.
Aqueous quantum dot ink provided by the invention can be to avoid addition containing only quanta point material and alcohol organic solvent
The introducing of agent, the influence to obtained quantum dot film charge transport ability.And due to the boiling point of the alcohol organic solvent compared with
Height volatilizees relatively slow at room temperature, the spray nozzle clogging caused by solvent volatilizees when can effectively avoid room temperature printing；But institute after inkjet printing
Stating alcohol organic solvent can fully be removed by heating or vacuum drying method, avoid the residual of alcohol organic solvent to preparing
Obtained film performance impacts.In addition, the present invention uses the aqueous quantum dot ink of alcohol organic solvent, viscosity, table
The parameters such as face tension also are adapted for inkjet printing requirement.
Specific implementation mode
In order to make technical problems, technical solutions and advantageous effects to be solved by the present invention be 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.
An embodiment of the present invention provides a kind of aqueous quantum dot ink, organic molten by quanta point material and at least one alcohols
Agent forms, and the boiling point of the alcohol organic solvent is 120 DEG C -280 DEG C, and the general structure of the alcohol organic solvent is R-
(OH)x, wherein the R is substituted or unsubstituted alkyl or cycloalkyl, and the x is positive integer.
Specifically, in the embodiment of the present invention, contains only quanta point material in the aqueous quantum dot ink and alcohols is organic
Solvent, and after inkjet printing forms a film, the alcohol organic solvent evaporative removal, formation charge can be passed from ink system
The good quantum dot film of defeated performance.
In the aqueous quantum dot ink, can only select a kind of alcohol organic solvent, can also use two kinds or
The two or more alcohol organic solvent, as long as the boiling point of the alcohol organic solvent meets 120 DEG C -280 DEG C.
Specifically, in the general structure of the alcohol organic solvent, the R is substituted or unsubstituted alkyl or cycloalkyl
The alkyl or cycloalkyl, i.e., the described R can be unsubstituted alkyl, or substitution alkyl；The R can be unsubstituted
Naphthenic base, or substituted cycloalkyl.
As a kind of implementation situation, the R is alkyl, and the general formula of the alkyl is ChH2h+2-x, wherein 1≤x≤h, institute
It includes branch saturated fat alkyl and straight chain saturated fat alkyl to state alkyl.Preferably, the amount of carbon atom of the alkyl is 5-
12, to ensure the boiling point of obtained alcohol organic solvent within the scope of 120 DEG C -280 DEG C.
As another implementation situation, the R is substitution alkyl.The substitution alkyl be on the basis of abovementioned alkyl,
One or more hydrogen atoms are substituted with a substituent to be formed.Wherein, the substituent group includes but not limited to alkyl, aryl.
As another implementation situation, the R is naphthenic base, and the general formula of the naphthenic base is CkH2k-x, wherein 1≤x≤
k.Preferably, the amount of carbon atom of the naphthenic base is 5-12, to ensure the boiling point of obtained alcohol organic solvent 120
Within the scope of DEG C -280 DEG C.
As another implementation situation, the R is substituted cycloalkyl.The substituted cycloalkyl is the base in above-mentioned naphthenic base
On plinth, one or more hydrogen atoms are substituted with a substituent to be formed.Wherein, the substituent group includes but not limited to alkyl, aryl.
Specifically, the alkyl includes but not limited to amyl, hexyl, heptyl, octyl, nonyl, decyl；The naphthenic base packet
Include but be not limited to cyclopenta, cyclohexyl, suberyl, cyclooctyl, cyclononyl, cyclodecyl.
In the embodiment of the present invention, the alcohol organic solvent can be monohydric alcohol.The monohydric alcohol preferably includes amylalcohol, different
Amylalcohol, sec-amyl alcohol, secondary isoamyl alcohol, 3- amylalcohols, tert-pentyl alcohol, cyclopentanol, 2- methyl anyl alcohols, 4- methyl -2- amylalcohols, n-hexyl alcohol, 2-
Hexanol, 2- methyl anyl alcohols, 2- methyl -2- amylalcohols, 2- methyl -3- amylalcohols, 3- ethyl -3- amylalcohols, n-heptanol, 2- enanthol, 3- heptan
Alcohol, 2-Ethylhexyl Alcohol, 2 methyl cyclohexanol, n-octyl alcohol, sec-n-octyl alcohol, 3,5,5- trimethyl hexanols, nonyl alcohol, 2,6- dimethyl -4-
Enanthol, Decanol, 5- ethyl -2- nonyl alcohols, undecyl alcohol, 5- ethyl -2- nonyl alcohols, dodecanol (laruyl alcohol), Exxal 12,
Cis- 2 methyl cyclohexanol, cis- 3 methyl cyclohexanol, cis- 4- methyl ring ethyl alcohol, butoxy ethanol, benzyl alcohol, benzhydrol,
Alpha-phenyl ethyl alcohol, bata-phenethyl alcohol.
In the embodiment of the present invention, the alcohol organic solvent can be dihydric alcohol.The dihydric alcohol preferably include ethylene glycol,
1,2- propylene glycol, 1,3- propylene glycol, 1,2- butanediols, 1,3 butylene glycol, 1,4- butanediols, 2,3- butanediols, 1,5- pentanediols,
2- methyl -2,4-PD, 2,2- dimethyl -1,3- propylene glycol, 2- butylene-1,4-diols, 2- methyl -2,4-PD, 2,
3- dimethyl -2,3- butanediols, 2- ethyl -1,3- hexylene glycols, 1,2,4- butantriols, 1,2,6- hexanetriols, pentaerythrite.
Under above-described embodiment situation, further the aqueous quantum can also be adjusted by adding low boiling point Organic Alcohol
The viscosity and surface tension of point ink, the low viscosity Organic Alcohol includes but not limited to the short carbon such as methanol, ethyl alcohol, propyl alcohol, butanol
Chain monohydric alcohol and propyl alcohol, butanol.
In the embodiment of the present invention, the quanta point material include II-VI group quanta point material, iii-v quanta point material,
Group IV-VI quanta point material.Further, in above-mentioned quanta point material, quantum-dot structure includes the uniform binary composition of quantum dot
The uniform multicomponent alloy component mononuclear structure of mononuclear structure, quantum dot, quantum dot multicomponent alloy content gradually variational mononuclear structure, quantum dot
The discrete nucleocapsid of binary composition, the discrete nucleocapsid of quantum dot multicomponent alloy group, quantum dot multicomponent alloy content gradually variational nucleocapsid
Structure.Further, one kind or one in materials described below can be used in the core in above-mentioned mononuclear structure, nucleocapsid and/or shell
Kind or more be made：CdSe, CdS of II-VI group, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS,
ZnSeTe、ZnTeS、CdSeS、CdSeTe、CdTeS、CdZnSeS、CdZnSeTe、CdZnSTe、CdSeSTe、ZnSeSTe、
CdZnSeSTe；InP, InAs, InAsP of iii-v；PbS, PbSe, PbTe, PbSeS, PbSeTe, PbSTe of group IV-VI.
Preferably, the quanta point material is aqueous quantum dot, and the ligand of the aqueous quantum dot is preferably sulfydryl acids
Or sulfydryl alcohols.Further, the sulfydryl acids ligand includes but not limited to thioacetic acid, 2 mercaptopropionic acid, 3- sulfydryls third
Acid, 3- mercaptobenzoic acids, 4- mercaptobenzoic acids, 6- mercaptohexanoic acids, dimercaptosuccinic acid, 11- Mercaptoundecanoic acids, 12- sulfydryls ten
Diacid, 16- mercaptohexadecanoic acids；The sulfydryl alcohols ligand includes but not limited to 2 mercapto ethanol, 1- thioglycerols, 2- sulfydryls-
3- butanol, 4- sulfydryls-n-butyl alcohol, 6- sulfydryl -1- hexanols, 8- sulfydryl -1- octanols, 9- sulfydryls -1 nonyl alcohol, 11- sulfydryls -1- 11
Alcohol.
In the embodiment of the present invention, by the total weight of the aqueous quantum dot ink be 100% in terms of, the quanta point material
Weight percentage is 0.01-20%, and the weight percentage of the alcohol organic solvent is 80-99.99%.Preferably, institute
The weight percentage for stating quanta point material is 0.4-6%.
Viscosity of the aqueous quantum dot ink that the embodiment of the present invention obtains under the conditions of 15-35 DEG C is 2-35cP, excellent
The range of viscosities of choosing is between 3-20cP, to be more suitable for inkjet printing.
Surface tension of the aqueous quantum dot ink that the embodiment of the present invention obtains under the conditions of 15-35 DEG C is 24-
45mN/m, preferred surface tension is between 26-36mN/m, to be more suitable for inkjet printing.
Aqueous quantum dot ink provided in an embodiment of the present invention can be kept away containing only quanta point material and alcohol organic solvent
The introducing for exempting from additive, the influence to obtained quantum dot film charge transport ability.And due to the alcohol organic solvent
Boiling point is higher, volatilizees at room temperature relatively slow, the spray nozzle clogging caused by solvent volatilizees when can effectively avoid room temperature printing；But ink-jet is beaten
The alcohol organic solvent can fully be removed by heating or vacuum drying method after print, avoid the residual of alcohol organic solvent
The film performance being prepared is impacted.In addition, aqueous quantum dot oil of the embodiment of the present invention using alcohol organic solvent
Ink, the parameters such as viscosity, surface tension also are adapted for inkjet printing requirement, can stablize during InkJet printing processes out of ink.
Aqueous quantum dot ink provided in an embodiment of the present invention, can be used as the electric ink of ink jet printing device, is particularly used in making
The photoelectric devices such as light emitting diode with quantum dots (QLED), quantum dot light power conversion device, quantum point sensor.
Aqueous quantum dot ink provided in an embodiment of the present invention, can be prepared by following methods.
Correspondingly, the embodiment of the present invention additionally provides a kind of preparation method of aqueous quantum dot ink, include the following steps：
S01. according to the formula of above-mentioned aqueous quantum dot ink, the quanta point material and alcohol organic solvent are provided.
S02. after adding the quanta point material in a reservoir, the alcohol organic solvent, oscillation stirring 20- is added
40min is particularly preferred as 30min, obtains aqueous quantum dot ink.
It is illustrated with reference to specific embodiment.
Embodiment 1
A kind of aqueous quantum dot ink, is made of, wherein the water water-soluble quantum dot and single solvent component n-heptanol
Dissolubility quantum dot is CdSe/ZnS water-soluble quantum dots, and ligand PEG, the weight percentage of the water-soluble quantum dot is
4%, the weight percentage of the n-heptanol is 96%.
The preparation method of the aqueous quantum dot ink includes the following steps：
Following components is added in 500mL single-necked flasks, order of addition is：8 grams of CdSe/ZnS water-soluble quantum dots,
233.6 milliliters i.e. 192 grams of n-heptanol solvent, oscillation stirring mixture 30 minutes, obtains 200 grams of quantum dot composition for ink.
Embodiment 2
A kind of aqueous quantum dot ink, is made of water-soluble quantum dot and binary mixed solvent, wherein the water-soluble amount
Son point is InP/ZnS water-soluble quantum dots, and ligand PEG, the binary mixed solvent is the mixing that ethylene glycol and ethyl alcohol form
Solvent, and the weight percentage of the water-soluble quantum dot is 4%, the weight percentage of the ethylene glycol is 80%, institute
The weight percentage for stating ethyl alcohol is 16%.
The preparation method of the aqueous quantum dot ink includes the following steps：
Following components is added in 500mL single-necked flasks, order of addition is：8 grams of InP/ZnS water-soluble quantum dots,
40.5 milliliters i.e. 32 grams of ethyl alcohol, oscillation stirring mixture 30 minutes, the ethylene glycol for then adding 142.9 milliliters i.e. 160 gram is molten
Agent, oscillation stirring mixture 10 minutes, obtains 200 grams of quantum dot composition for ink.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of aqueous quantum dot ink, which is characterized in that be made of quanta point material and at least one alcohol organic solvent, institute
The boiling point for stating alcohol organic solvent is 120 DEG C -280 DEG C, and the general structure of the alcohol organic solvent is R- (OH)x, wherein institute
It is substituted or unsubstituted alkyl or cycloalkyl to state R, and the x is positive integer.
2. aqueous quantum dot ink as described in claim 1, which is characterized in that the amount of carbon atom of the alkyl or cycloalkyl
For 5-12.
3. aqueous quantum dot ink as described in claim 1, which is characterized in that in the substituted alkyl or cycloalkyl, take
Dai Ji includes alkyl, aryl.
4. aqueous quantum dot ink as described in claim 1, which is characterized in that the alkyl include amyl, hexyl, heptyl,
Octyl, nonyl, decyl；The naphthenic base includes cyclopenta, cyclohexyl, suberyl, cyclooctyl, cyclononyl, cyclodecyl.
5. aqueous quantum dot ink as described in claim 1, which is characterized in that the alcohol organic solvent is monohydric alcohol, institute
It includes amylalcohol, isoamyl alcohol, sec-amyl alcohol, secondary isoamyl alcohol, 3- amylalcohols, tert-pentyl alcohol, cyclopentanol, 2- methyl anyl alcohols, 4- first to state monohydric alcohol
Base -2- amylalcohols, n-hexyl alcohol, 2- hexanols, 2- methyl anyl alcohols, 2- methyl -2- amylalcohols, 2- methyl -3- amylalcohols, 3- ethyl -3- amylalcohols,
N-heptanol, 2- enanthol, 3- enanthol, 2-Ethylhexyl Alcohol, 2 methyl cyclohexanol, n-octyl alcohol, sec-n-octyl alcohol, 3,5,5- trimethyl hexanols,
Nonyl alcohol, 2,6- 2,6-dimethyl-4-heptanols, Decanol, 5- ethyl -2- nonyl alcohols, undecyl alcohol, 5- ethyl -2- nonyl alcohols, the dodecanol (moon
Cinnamic alcohol), Exxal 12, cis- 2 methyl cyclohexanol, cis- 3 methyl cyclohexanol, cis- 4- methyl ring ethyl alcohol, 2- butoxy second
Alcohol, benzyl alcohol, benzhydrol, alpha-phenyl ethyl alcohol, bata-phenethyl alcohol.
6. aqueous quantum dot ink as described in claim 1, which is characterized in that the alcohol organic solvent is dihydric alcohol, institute
It includes ethylene glycol, 1,2- propylene glycol, 1,3- propylene glycol, 1,2- butanediols, 1,3 butylene glycol, 1,4- butanediols, 2 to state dihydric alcohol,
3- butanediols, 1,5- pentanediols, 2- methyl -2,4-PD, 2,2- dimethyl -1,3- propylene glycol, 2- butylene-1,4-diols,
2- methyl -2,4-PD, 2,3- dimethyl -2,3- butanediols, 2- ethyl -1,3- hexylene glycols, 1,2,4- butantriols, 1,2,6-
Hexanetriol, pentaerythrite.
7. aqueous quantum dot ink as described in claim 1, which is characterized in that the aqueous quantum dot ink is at 15-35 DEG C
Under the conditions of viscosity be 2-35cP.
8. aqueous quantum dot ink as described in claim 1, which is characterized in that the aqueous quantum dot ink is at 15-35 DEG C
Under the conditions of surface tension be 24-45mN/m.
9. the aqueous quantum dot ink as described in claim 1-8 is any, which is characterized in that with the aqueous quantum dot ink
Total weight is 100% meter, and the weight percentage of the quanta point material is 0.01-20%, the weight of the alcohol organic solvent
Amount percentage composition is 80-99.99%.
10. the aqueous quantum dot ink as described in claim 1-8 is any, which is characterized in that the quanta point material includes II-
VI races quanta point material, iii-v quanta point material, group IV-VI quanta point material.
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| CN201710176903.9A CN108624137A (en) | 2017-03-22 | 2017-03-22 | Aqueous quantum dot ink |
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Cited By (4)
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| CN109735168A (en) * | 2018-03-23 | 2019-05-10 | 广东聚华印刷显示技术有限公司 | Cycloalkane alcohol is preparing the application in quantum dot ink, quantum dot ink and preparation method thereof as additive |
| CN110564404A (en) * | 2019-08-30 | 2019-12-13 | 苏州星烁纳米科技有限公司 | Preparation method of quantum dot, quantum dot composition and color film |
| CN111384307A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN115851038A (en) * | 2022-12-26 | 2023-03-28 | 北京印刷学院 | Ternary solvent-based red quantum dot ink-jet ink and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735168A (en) * | 2018-03-23 | 2019-05-10 | 广东聚华印刷显示技术有限公司 | Cycloalkane alcohol is preparing the application in quantum dot ink, quantum dot ink and preparation method thereof as additive |
| CN109735168B (en) * | 2018-03-23 | 2022-03-18 | 广东聚华印刷显示技术有限公司 | Application of cyclanol as additive in preparation of quantum dot ink, quantum dot ink and preparation method of quantum dot ink |
| CN111384307A (en) * | 2018-12-29 | 2020-07-07 | Tcl集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| CN111384307B (en) * | 2018-12-29 | 2021-04-09 | Tcl科技集团股份有限公司 | Preparation method of quantum dot light-emitting diode |
| US11889745B2 (en) | 2018-12-29 | 2024-01-30 | Tcl Technology Group Corporation | QLED manufacturing method |
| CN110564404A (en) * | 2019-08-30 | 2019-12-13 | 苏州星烁纳米科技有限公司 | Preparation method of quantum dot, quantum dot composition and color film |
| CN115851038A (en) * | 2022-12-26 | 2023-03-28 | 北京印刷学院 | Ternary solvent-based red quantum dot ink-jet ink and preparation method thereof |
| CN115851038B (en) * | 2022-12-26 | 2024-01-16 | 北京印刷学院 | Red quantum dot ink-jet ink based on ternary solvent and preparation method thereof |
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