CN106566316A - Quantum dot ink and preparation method thereof - Google Patents
Quantum dot ink and preparation method thereof Download PDFInfo
- Publication number
- CN106566316A CN106566316A CN201610936155.5A CN201610936155A CN106566316A CN 106566316 A CN106566316 A CN 106566316A CN 201610936155 A CN201610936155 A CN 201610936155A CN 106566316 A CN106566316 A CN 106566316A
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- Prior art keywords
- quantum dot
- solvent
- ether
- dot ink
- glycol
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
Abstract
The invention discloses quantum dot ink and a preparation method thereof. The quantum dot ink comprises the following components by weight percentage: 0.01-20.0% of quantum dots and 80.0-99.99% of solvent, wherein the solvent comprises at least one halogenating aromatic solvent and at least one alcohol ether solvent, and the dosage of the halogenating aromatic solvent is 50-95% of the total weight of the solvent. With the adoption of the formula, the obtained quantum dot ink has appropriate parameters, and can meet the requirements of an ink-jet printing technology on the quantum dot ink. With the adoption of the quantum dot ink, ink can be discharged stably in an ink-jet printing technical process; in addition, the halogenating aromatic solvent and the alcohol ether solvent have high boiling points, and have low volatility under room temperature condition, so that nozzle blocking of a printing head caused by solvent volatilization in a non-operating state can be reduced. In addition, the solvent can be removed in a vacuum evaporation or heating evaporation mode and the like, so that a film of a quantum dot material is formed.
Description
Technical field
The present invention relates to quantum dot ink set field, more particularly to a kind of quantum dot ink and preparation method thereof.
Background technology
Semiconductor-quantum-point lights with light excitation height, luminous quantum efficiency is high, glow color is adjustable, long service life
Deng good characteristic.These features cause the light emitting diode with quantum dots using quanta point material as luminescent layer（QLED）Shine in solid-state
The fields such as bright, FPD are with a wide range of applications, and receive the extensive concern of academia and industrial circle.
Quantum dot is dispersed among being configured to the printing materials such as quantum dot ink in solvent, it is adaptable to which prepared by solwution method, can adopt
Quantum dot film is manufactured with methods such as printing, bat printing, spin coatings.
Inkjet printing（Ink-jet printing）Technology in recent years opto-electronic device manufacture obtain extensive research and
Using, particularly as flat-panel display device, such as OLED and QLED show manufacturing technology in be considered as solve high cost and
Realize large-area effective way, this technology can with reference to the functional material and advanced ink jet printing device based on solution 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.But spray
Black printing device requires ink higher, such as appropriate viscosity, surface tension, boiling point and evaporation rate and is uniformly dispersed stable
Solute, bring larger difficulty to ink formulation.
Quantum dot is usually dispersed in short carbon chain alkane or monocyclic aromatic equal solvent, for example octane, hexane, toluene etc.
Solvent, viscosity under the conditions of these solvent room temperatures, boiling point is relatively low and evaporation rate is too fast.Using this low viscous solvent, ink-jet
Ink droplet is wayward in print procedure, and under non-print holding state, easily causes solvent volatilization and cause quantum dot in nozzle
Aggregation causes blocking.
In prior art, in order to regulate and control the physical parameter of ink, these quantum dot inks all include other additives,
Such as alcohols polymer.Alcohols polymer with insulating property (properties) is difficult to remove, and this kind of polymer of introducing often reduces film
Charge transport ability, there is negative effect to the photoelectric properties of device.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of quantum dot ink and its preparation side
Method, it is intended to solve that existing quantum dot solution viscosity is too low to cause to print that unstable, evaporation rate is too fast causes nozzle easily to block
And solve the problems, such as that the introducing of quantum dot ink is difficult to remove additive.
Technical scheme is as follows：
A kind of quantum dot ink, wherein, by weight percentage, including following component：
Quantum dot：0.01-20.0%；
Solvent：80.0-99.99%；Wherein, the solvent includes at least one Polyhalogenated aromatic hydrocarbons solvent and at least one alcohol ether
Class solvent, the consumption of the Polyhalogenated aromatic hydrocarbons solvent is the 50-95% of solvent gross weight.
Described quantum dot ink, wherein, the boiling spread of the Polyhalogenated aromatic hydrocarbons solvent is 150 DEG C -230 DEG C, institute
The boiling spread for stating alcohol ethers solvent is 120 DEG C -280 DEG C.
Described quantum dot ink, wherein, the range of viscosities of the quantum dot ink is 1cP-40cP.
Described quantum dot ink, wherein, the surface tension range of the quantum dot ink is 25-50mN/m.
Described quantum dot ink, wherein, the Polyhalogenated aromatic hydrocarbons solvent be bromobenzene, iodobenzene, 1,2- dichloro-benzenes, 1,3-
One kind in dichloro-benzenes, 1,2- dibromobenzenes 225,1,3- dibromobenzenes, ortho-chlorotolu'ene, parachlorotoluene, o-bromotoluene, parabromotoluene or
It is various.
Described quantum dot ink, wherein, the alcohol ethers solvent is EGME, ethylene glycol ethyl ether, ethylene glycol third
Ether, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, Propylene glycol n-propyl ether, propane diols isopropyl ether, propylene glycol n-butyl ether, third
The tertiary butyl ether of glycol, diethylene glycol ether, diethylene glycol dimethyl ether, diethylene glycol dimethyl ether, diethylene glycol ether, diethylene glycol diethyl
Ether, butyl, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, dipropylene glycol methyl ether, dimethyl ether, dipropyl
2-ethoxyethanol, dipropylene glycol diethyl ether, dipropylene, tri ethylene glycol ethyl ether, tripropylene glycol methyl ether, tripropylene glycol butyl ether
In one or more.
Described quantum dot ink, wherein, the consumption of the Polyhalogenated aromatic hydrocarbons solvent is the 60-90% of solvent gross weight.
Described quantum dot ink, wherein, the consumption of the quantum dot is the 0.8-12% of quantum dot ink gross weight.
Described quantum dot ink, wherein, the quantum dot is II- IV compound semiconductors, III-V or IV-VI
One kind in compound semiconductor, I-III-VI2 races semiconductor nano.
A kind of preparation method of as above arbitrary described quantum dot ink, wherein, including step：
A, according to above-mentioned formula, under agitation, quantum dot is dispersed in Polyhalogenated aromatic hydrocarbons solvent；
B, again under agitation, adds alcohol ethers solvent, obtains quantum dot ink.
Beneficial effect：The solvent that the present invention is adopted has higher boiling point, not volatile under room temperature, can avoid because solvent is waved
Send out and cause spray nozzle clogging；Simultaneously the parameter such as quantum dot ink viscosity, surface tension also is adapted for inkjet printing requirement, owns in addition
Solvent can be removed using the method such as heating or vacuum drying.
Specific embodiment
The present invention provides a kind of quantum dot ink and preparation method thereof, to make the purpose of the present invention, technical scheme and effect
Clearer, clear and definite, below the present invention is described in more detail.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
The present invention provides a kind of quantum dot ink, its by weight percentage, including following component：Quantum dot：0.01-
20.0%；Solvent：80.0-99.99%；Wherein, the solvent includes at least one Polyhalogenated aromatic hydrocarbons solvent and at least one alcohol
Ether solvent, the consumption of the Polyhalogenated aromatic hydrocarbons solvent is the 50-95% of solvent gross weight.Preferably, the use of the quantum dot
Measure as the 0.8-12% of quantum dot ink gross weight, the consumption of the Polyhalogenated aromatic hydrocarbons solvent for solvent gross weight 60-90%.
The present invention adopts above-mentioned formula, the quantum dot ink of acquisition to have suitable parameter, can meet the requirement of inkjet printing.
Specifically, the solvent that quantum dot ink of the present invention is used is comprising at least one Polyhalogenated aromatic hydrocarbons solvent and at least
A kind of alcohol ethers solvent.The boiling spread of the Polyhalogenated aromatic hydrocarbons solvent is 150 DEG C -230 DEG C, the boiling of the alcohol ethers solvent
Point range is 120 DEG C -280 DEG C.The Polyhalogenated aromatic hydrocarbons solvent and alcohol ethers solvent can evaporate from dicyandiamide solution, to be formed
CdS quantum dots film.Above-mentioned solvent can be removed using the method such as heating or vacuum drying.
Specifically, at ambient temperature, the range of viscosities of quantum dot ink of the present invention is 1cP-40cP, it is preferable that
Range of viscosities is 2cP-20cP.At ambient temperature, the surface tension range of the quantum dot ink is 25-50mN/m, preferably
Ground, surface tension range is 25-40mN/m.The viscosity and surface tension of quantum dot ink of the present invention is suitable for inkjet printing will
Ask.
Polyhalogenated aromatic hydrocarbons solvent of the present invention, i.e. halogen atom is connected on aromatic ring carbon atom.For example, halogenated aromatic
Varsol can be but be not limited to bromobenzene, iodobenzene, 1,2- dichloro-benzenes, 1,3- dichloro-benzenes, 1,2- dibromobenzenes 225,1,3- dibromos
One or more in benzene, ortho-chlorotolu'ene, parachlorotoluene, o-bromotoluene, parabromotoluene.
Preferably, the alcohol ethers solvent it is characterized by this kind of solvent at least one ehter bond-O- and alcoholic extract hydroxyl group-
OH, comprising dihydroxylic alcohols ether solvent and polyalcohol ether solvent.The alcohol ethers solvent can be but be not limited to EGME,
Ethylene glycol ethyl ether, glycol propyl ether, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, Propylene glycol n-propyl ether, propane diols are different
Propyl ether, propylene glycol n-butyl ether, glycol tertiary butyl ether, diethylene glycol ether, diethylene glycol dimethyl ether, diethylene glycol dimethyl ether, diethyl two
Alcohol ether, diethylene glycol diethyl ether, butyl, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, dipropylene glycol methyl ether,
Dimethyl ether, DPE, dipropylene glycol diethyl ether, dipropylene, tri ethylene glycol ethyl ether, 3 the third two
One or more in alcohol methyl ether, tripropylene glycol butyl ether.
Preferably, the quantum dot can be II-IV compound semiconductors（Such as CdS, CdSe, CdS/ZnS, CdSe/
ZnS or CdSe/CdS/ZnS）, can also be III-V or group IV-VI compound semiconductor（Such as GaAs, InP, PbS/ZnS or
PbSe/ZnS）And the one kind in the semiconductor nano such as I-III-VI2 races.
Preferably, the average-size of the quantum dot is 2 ~ 20nm.And the quantum dot can be homogeneous mixed type,
Gradient mixed type, core-shell structure copolymer type or union type.The quantum dot can be oil-soluble quantum dot.The quantum dot is selected from
Doped or non-doped quantum dot.
Preferably, the part of the quantum dot can for sour part, mercaptan part, amine ligand,（Oxygen）Phosphine ligands, phosphatide,
One or more in soft phosphatide, polyvinylpyridine.The sour part includes ten acid, undecenoic acid, tetradecylic acid, oleic acid and firmly
One or more in resin acid；The mercaptan part is included in eight alkyl hydrosulfides, lauryl mercaptan and Stearyl mercaptan
One or more；The amine ligand includes one or more in oleyl amine, octadecylamine and eight amine；It is described（Oxygen）Phosphine ligands include three
One or more of octyl group phosphine, trioctylphosphine oxide (TOPO).
Based on above-mentioned quantum dot ink, the present invention also provides the preparation side of a kind of as above arbitrary described quantum dot ink
Method, it includes step：
A, according to above-mentioned formula, under agitation, quantum dot is dispersed in Polyhalogenated aromatic hydrocarbons solvent；
B, again under agitation, adds alcohol ethers solvent, obtains quantum dot ink.
The solvent that the present invention is adopted has higher boiling point, not volatile under room temperature, can avoid causing because solvent volatilizees
Spray nozzle clogging；Simultaneously the parameter such as quantum dot ink viscosity, surface tension also is adapted for inkjet printing requirement, and in addition all solvents can be adopted
Removed with the method such as heating or vacuum drying.
It is further described that (wt% is weight percentage to the present invention below by embodiment）.
Embodiment 1
Quantum dot ink is made up of CdSe/ZnS oil-soluble quantum dots, 1,2- dichloro-benzenes, diethylene glycol dimethyl ether.Wherein, CdSe/
The percentage by weight of ZnS oil-soluble quantum dots is 5%, and the percentage by weight of 1,2- dichloro-benzenes is the weight of 70%, diethylene glycol dimethyl ether
Amount percentage is 25%.
Following components is added in 500mL single-necked flasks, in the case of stirring, order of addition is：5wt%'s
CdSe/ZnS oil-soluble quantum dots, 1, the 2- dichloro benzene solvents of 70wt%, the diethylene glycol dimethyl ether solvent of 25wt %, stirring mixing
Thing 30 minutes, obtains quantum dot ink.
Embodiment 2
Quantum dot ink is made up of CdSe/CdS/ZnS oil-soluble quantum dots, bromobenzene, diethylene glycol ether.Wherein, CdSe/CdS/
The percentage by weight of ZnS oil-soluble quantum dots is 1%, and the percentage by weight of bromobenzene is the weight percent of 64%, diethylene glycol ether
Than for 35%.
Following components is added in 500mL single-necked flasks, in the case of stirring, order of addition is：1wt%'s
CdSe/CdS/ZnS oil-soluble quantum dots, the bromobenzene solvent of 64wt%, the diethylene glycol ether solvent of 35wt%, stirring mixture 30
Minute, obtain quantum dot ink.
In sum, quantum dot ink of inkjet printing that the present invention is provided and preparation method thereof, by weight percentage
Meter, including following component：Quantum dot：0.01-20.0%；Solvent：80.0-99.99%；Wherein, the solvent includes at least one
Polyhalogenated aromatic hydrocarbons solvent and at least one alcohol ethers solvent, the consumption of the Polyhalogenated aromatic hydrocarbons solvent is solvent gross weight
50-95%.The present invention adopts above-mentioned formula, the quantum dot ink of acquisition to have suitable parameter, disclosure satisfy that inkjet technology
Requirement to quantum dot ink.Can stablize out of ink during InkJet printing processes using the quantum dot ink；While halogen
There is higher boiling point for aromatic hydrocarbon and alcohol ethers solvent, at ambient temperature volatility is less, can reduce printhead non-
Solvent volatilization under working condition causes spray nozzle clogging.In addition, solvent can be removed by modes such as vacuum evaporation or heating evaporations,
To form the film of quanta point material.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, and for those of ordinary skills, can
To be improved according to the above description or be converted, all these modifications and variations should all belong to the guarantor of claims of the present invention
Shield scope.
Claims (10)
1. a kind of quantum dot ink, it is characterised in that by weight percentage, including following component：
Quantum dot：0.01-20.0%；
Solvent：80.0-99.99%；Wherein, the solvent includes at least one Polyhalogenated aromatic hydrocarbons solvent and at least one alcohol ether
Class solvent, the consumption of the Polyhalogenated aromatic hydrocarbons solvent is the 50-95% of solvent gross weight.
2. quantum dot ink according to claim 1, it is characterised in that the boiling spread of the Polyhalogenated aromatic hydrocarbons solvent
For 150 DEG C -230 DEG C, the boiling spread of the alcohol ethers solvent is 120 DEG C -280 DEG C.
3. quantum dot ink according to claim 1, it is characterised in that the range of viscosities of the quantum dot ink is 1cP-
40cP。
4. quantum dot ink according to claim 1, it is characterised in that the surface tension range of the quantum dot ink is
25-50mN/m。
5. quantum dot ink according to claim 1, it is characterised in that the Polyhalogenated aromatic hydrocarbons solvent is bromobenzene, iodine
Benzene, 1,2- dichloro-benzenes, 1,3- dichloro-benzenes, 1,2- dibromobenzenes 225,1,3- dibromobenzenes, ortho-chlorotolu'ene, parachlorotoluene, o-bromotoluene,
One or more in parabromotoluene.
6. quantum dot ink according to claim 1, it is characterised in that the alcohol ethers solvent is EGME, second
Glycol ether, glycol propyl ether, butyl glycol ether, propylene glycol monomethyl ether, propylene-glycol ethyl ether, Propylene glycol n-propyl ether, propane diols isopropyl
Ether, propylene glycol n-butyl ether, glycol tertiary butyl ether, diethylene glycol ether, diethylene glycol dimethyl ether, diethylene glycol dimethyl ether, diethylene glycol
Ether, diethylene glycol diethyl ether, butyl, dibutyl ethylene glycol ether, diethylene glycol hexyl ether, dipropylene glycol methyl ether, two
Propylene Glycol Dimethyl Ether, DPE, dipropylene glycol diethyl ether, dipropylene, tri ethylene glycol ethyl ether, tripropylene glycol
One or more in methyl ether, tripropylene glycol butyl ether.
7. quantum dot ink according to claim 1, it is characterised in that the consumption of the Polyhalogenated aromatic hydrocarbons solvent is molten
The 60-90% of agent gross weight.
8. quantum dot ink according to claim 1, it is characterised in that the consumption of the quantum dot is that quantum dot ink is total
The 0.8-12% of weight.
9. quantum dot ink according to claim 1, it is characterised in that the quantum dot is II- IV compounds of group half
One kind in conductor, III-V or IV-VI compound semiconductors, I-III-VI2 races semiconductor nano.
10. a kind of preparation method of the quantum dot ink as described in claim 1 ~ 9 is arbitrary, it is characterised in that including step：
A, according to above-mentioned formula, under agitation, quantum dot is dispersed in Polyhalogenated aromatic hydrocarbons solvent；
B, again under agitation, adds alcohol ethers solvent, obtains quantum dot ink.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610936155.5A CN106566316A (en) | 2016-11-01 | 2016-11-01 | Quantum dot ink and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610936155.5A CN106566316A (en) | 2016-11-01 | 2016-11-01 | Quantum dot ink and preparation method thereof |
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| CN106566316A true CN106566316A (en) | 2017-04-19 |
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| CN201610936155.5A Pending CN106566316A (en) | 2016-11-01 | 2016-11-01 | Quantum dot ink and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810571A (en) * | 2017-11-21 | 2019-05-28 | Tcl集团股份有限公司 | Inorganic nano material prints ink and its preparation method and application |
| CN110079159A (en) * | 2018-04-28 | 2019-08-02 | 广东聚华印刷显示技术有限公司 | Quantum dot ink and preparation method thereof |
| RU2720778C2 (en) * | 2018-09-28 | 2020-05-13 | Владислав Юрьевич Мирчев | Ink with quantum dots for digital piezo-jet printing and method of application thereof |
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| CN105062218A (en) * | 2015-08-21 | 2015-11-18 | Tcl集团股份有限公司 | Quantum dot printing ink for ink-jet printing and preparation method thereof |
| CN105131712A (en) * | 2015-07-28 | 2015-12-09 | Tcl集团股份有限公司 | Quantum dot printing ink and preparation method thereof, and quantum dot light emitting diode |
| CN105820662A (en) * | 2016-04-26 | 2016-08-03 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
| CN105907180A (en) * | 2016-05-04 | 2016-08-31 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
-
2016
- 2016-11-01 CN CN201610936155.5A patent/CN106566316A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131712A (en) * | 2015-07-28 | 2015-12-09 | Tcl集团股份有限公司 | Quantum dot printing ink and preparation method thereof, and quantum dot light emitting diode |
| CN105062218A (en) * | 2015-08-21 | 2015-11-18 | Tcl集团股份有限公司 | Quantum dot printing ink for ink-jet printing and preparation method thereof |
| CN105820662A (en) * | 2016-04-26 | 2016-08-03 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
| CN105907180A (en) * | 2016-05-04 | 2016-08-31 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810571A (en) * | 2017-11-21 | 2019-05-28 | Tcl集团股份有限公司 | Inorganic nano material prints ink and its preparation method and application |
| CN110079159A (en) * | 2018-04-28 | 2019-08-02 | 广东聚华印刷显示技术有限公司 | Quantum dot ink and preparation method thereof |
| RU2720778C2 (en) * | 2018-09-28 | 2020-05-13 | Владислав Юрьевич Мирчев | Ink with quantum dots for digital piezo-jet printing and method of application thereof |
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Application publication date: 20170419 |