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WO2017161629A1 - 量子点打印墨水的制作方法及制得的量子点打印墨水 - Google Patents

量子点打印墨水的制作方法及制得的量子点打印墨水 Download PDF

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WO2017161629A1
WO2017161629A1 PCT/CN2016/080282 CN2016080282W WO2017161629A1 WO 2017161629 A1 WO2017161629 A1 WO 2017161629A1 CN 2016080282 W CN2016080282 W CN 2016080282W WO 2017161629 A1 WO2017161629 A1 WO 2017161629A1
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solvent
quantum dot
printing ink
dot printing
cps
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PCT/CN2016/080282
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English (en)
French (fr)
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刘亚伟
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深圳市华星光电技术有限公司
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Priority to US15/108,321 priority Critical patent/US10246598B2/en
Publication of WO2017161629A1 publication Critical patent/WO2017161629A1/zh

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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
    • C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/033—Printing inks characterised by features other than the chemical nature of the binder characterised by the solvent
    • 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
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • 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
    • C09D11/32—Inkjet printing inks characterised by colouring agents
    • C09D11/322—Pigment 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
    • C09D11/50—Sympathetic, colour changing or similar 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
    • C09D11/52—Electrically conductive inks
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
    • C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
    • Y10S977/774—Exhibiting three-dimensional carrier confinement, e.g. quantum dots
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/70—Nanostructure
    • Y10S977/778—Nanostructure within specified host or matrix material, e.g. nanocomposite films
    • Y10S977/786—Fluidic host/matrix containing nanomaterials
    • Y10S977/787—Viscous fluid host/matrix containing nanomaterials
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/90—Manufacture, treatment, or detection of nanostructure having step or means utilizing mechanical or thermal property, e.g. pressure, heat
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/902—Specified use of nanostructure
    • Y10S977/932—Specified use of nanostructure for electronic or optoelectronic application
    • Y10S977/949—Radiation emitter using nanostructure
    • Y10S977/95—Electromagnetic energy

Definitions

  • the present invention relates to the field of display technologies, and in particular, to a method for fabricating a quantum dot printing ink and a quantum dot printing ink produced.
  • NCs Semiconductor nanocrystals
  • QDs quantum dots
  • Quantum Dots Light Emitting Diodes have important commercial applications and have attracted strong research interest in the last decade. In fact, QD-LEDs have many advantages over Organic Light Emitting Diodes (OLEDs): (1) The line width of quantum dot luminescence is between 20-30 nm, relative to the luminescence of organic luminescence >50 nm, half FWHM (full width at half maximum) is narrow, which plays a key role in the color purity of realistic images; (2) inorganic materials exhibit better thermal stability relative to organic materials when the device is in high brightness or At high current densities, Joule heat is the main cause of device degradation.
  • OLEDs Organic Light Emitting Diodes
  • the limit of the organic fluorescent dye ⁇ r is 25%, wherein the ratio of the singlet to the triplet is 1:3, and only the combination of singlet excitons leads to luminescence, however, due to the spin-orbit coupling, the ⁇ of the organic phosphorescent material r is greater than 25%.
  • the organic phosphorescent material causes degradation of the matrix material, and the ⁇ OUT of the planar light-emitting device is about 20%, which can improve the outcoupling efficiency through the microcavity structure.
  • ⁇ INT can reach 100%, and when the electron and hole levels are suitable at the same time, ⁇ r can also reach 100%.
  • Ink-jet printing is a non-contact, pressure-free, non-printing printing technology that has the common feature of non-printing digital printing and enables printing of various inks.
  • the basic principle is to input the graphic information stored by the computer to the flatbed printer first, and then, through a special device, under the control of the electronic computer, the ink droplets are ejected from the nozzle to the surface of the substrate, and the ink droplets are spread out and dried. And forming a film at the desired location.
  • the quantum dot material can be formulated into ink and inkjet printing technology can be used for thin film device preparation.
  • inkjet printing technology the viscosity and surface tension of the ink are usually adjusted. It is common practice to add a surfactant, but when the ink is dried, if a surfactant remains in the film, The performance of the film has an adverse effect, and the surfactant is equivalent to an impurity in the film, which has an influence on the conductivity and luminescence properties of the film.
  • the object of the present invention is to provide a method for fabricating a quantum dot printing ink, which is prepared by mixing a plurality of solvents to prepare a quantum dot printing ink having properties such as viscosity, surface tension and drying conditions, which are suitable for inkjet printing, and avoid adding in ink.
  • the surfactant which is obtained by ink-jet printing the quantum dot printing ink, does not contain a surfactant, thereby avoiding influence on the conductivity and luminescent properties of the film.
  • Another object of the present invention is to provide a quantum dot printing ink which does not contain a surfactant.
  • the film obtained by ink jet printing of the ink does not contain a surfactant, and has good conductivity and luminescent properties.
  • the present invention provides a method of fabricating a quantum dot printing ink, comprising the steps of:
  • Step 1 providing a quantum dot material and a first solvent, mixing the quantum dot material with the first solvent, and uniformly dispersing to obtain a first mixed solution;
  • Step 2 providing a second solvent that is miscible with the first solvent, adding the second solvent to the first mixed solution according to a ratio of the first solvent to the second solvent in a volume ratio of 1:2 to 2:1. Mixing uniformly to obtain a second mixed solution having a viscosity of between 1 and 10 cps;
  • Step 3 providing a third solvent that is miscible with the first and second solvents, according to the first solvent and the second solvent
  • the ratio of the sum of the solvent to the third solvent is 1:2 to 2:1
  • the third solvent is added to the second mixed solution, and the mixture is uniformly mixed to obtain a viscosity of 1 to 10 cps, and the surface tension is Quantum dot printing ink between 30 and 40 dyne/cm.
  • step 4 providing a fourth solvent miscible with the first, second, and third solvents, according to a ratio of the fourth solvent to the sum of the first, second, and third solvents, a ratio of less than 1/9,
  • the four solvents are added to the quantum dot printing ink, and the mixture is uniformly mixed.
  • the viscosity of the quantum dot printing ink is maintained between 1 and 10 cps, and the surface tension is between 30 and 40 dyne/cm, and the room temperature vapor pressure of the quantum dot printing ink is adjusted. Up to 100mmHg or less.
  • the viscosity of the first solvent and the second solvent may not both be less than 1 cps, and may not be greater than 10 cps.
  • the first solvent is monoethylene glycol; the second solvent is n-butanol; the third solvent is methylpyrrolidone; and the fourth solvent is propylene glycol propyl ether.
  • the quantum dot material has a mass percentage concentration of 0.1 wt% to 10 wt%.
  • the present invention also provides a quantum dot printing ink comprising a quantum dot material, and a mutually soluble first solvent, a second solvent and a third solvent, wherein the volume ratio of the first solvent to the second solvent is 1:2 to 2: 1.
  • the volume ratio of the sum of the first solvent and the second solvent to the third solvent is 1:2 to 2:1, the viscosity of the quantum dot printing ink is between 1 and 10 cps, and the surface tension is between 30 and 40 dyne. Between /cm.
  • the volume ratio of the fourth solvent to the sum of the first, second, and third solvents being less than 1/9, such that the quantum dot printing ink
  • the room temperature vapor pressure is below 100 mmHg.
  • the viscosity of the first solvent and the second solvent may not both be less than 1 cps, and may not be greater than 10 cps.
  • the first solvent is monoethylene glycol; the second solvent is n-butanol; the third solvent is methylpyrrolidone; and the fourth solvent is propylene glycol propyl ether.
  • the quantum dot material has a mass percentage concentration of 0.1 wt% to 10 wt%.
  • the present invention also provides a quantum dot printing ink comprising a quantum dot material, and a mutually soluble first solvent, a second solvent and a third solvent, wherein the volume ratio of the first solvent to the second solvent is 1:2 to 2: 1.
  • the volume ratio of the sum of the first solvent and the second solvent to the third solvent is 1:2 to 2:1, the viscosity of the quantum dot printing ink is between 1 and 10 cps, and the surface tension is between 30 and 40 dyne. Between /cm;
  • the viscosity of the first solvent and the second solvent may not be less than 1 cps, and may not be greater than 10 cps;
  • the quantum dot material has a mass percentage concentration of 0.1 wt% to 10 wt%.
  • the present invention provides a method for fabricating a quantum dot printing ink, which adjusts the viscosity of the quantum dot printing ink to a desired range by mixing the first solvent with the second solvent, and then passes through the third solvent and The mixing of the first and second solvents adjusts the surface tension of the quantum dot printing ink to a desired range while maintaining the viscosity of the quantum dot printing ink within a predetermined range, and further, by adding the quantum dot printing ink
  • the fourth solvent is used to adjust the vapor pressure to a reasonable range.
  • a quantum dot printing ink suitable for inkjet printing such as viscosity, surface tension, and drying conditions
  • the surfactant is added, and the film obtained by ink-jet printing the quantum dot printing ink does not contain a surfactant, thereby avoiding influence on the conductivity and luminescence properties of the film.
  • the invention provides a quantum dot printing ink comprising a plurality of mixed solvents, which is suitable for inkjet printing quantum dot printing inks with properties such as viscosity, surface tension and drying conditions, and the ink does not contain a surfactant, and is inkjet.
  • the film obtained by printing the ink does not contain a surfactant, and has good electrical conductivity and luminescent properties.
  • 1 is a flow chart of a method of fabricating a quantum dot printing ink of the present invention.
  • the present invention provides a method for fabricating a quantum dot printing ink, comprising the following steps:
  • Step 1 Providing a quantum dot material and a first solvent, mixing the quantum dot material with the first solvent, and uniformly dispersing to obtain a first mixed solution.
  • the quantum dot material may be a nanocrystal of a group II-VI, a group III-V, a group IV element or a compound thereof.
  • the quantum dot material may be a hole injecting layer (HIL layer) material, a hole transporting layer (HTL) material, an emission layer (EML) material, or an electron transport. Electron transporting layer (ETL) material.
  • HIL layer hole injecting layer
  • HTL hole transporting layer
  • EML emission layer
  • ETL electron transport.
  • ETL Electron transporting layer
  • the quantum dot material is uniformly dispersed in the first solvent by stirring and ultrasonic vibration to obtain a first mixed solution.
  • Step 2 providing a second solvent that is miscible with the first solvent, adding the second solvent to the first mixed solution according to a ratio of the first solvent to the second solvent in a volume ratio of 1:2 to 2:1.
  • the mixture was uniformly mixed to obtain a second mixed solution having a viscosity of from 1 to 10 cps.
  • the viscosity of the first solvent and the second solvent may not be less than 1 cps, and may not be greater than 10 cps.
  • the viscosity of the second mixed solution is adjusted to be between 1 and 10 cps by adjusting the volume ratio of the first solvent to the second solvent.
  • the volume ratio of the first solvent to the second solvent is 2:1, 1:1, or 1:2, and the like.
  • the second solvent is uniformly mixed with the first mixed solution by stirring to obtain a second mixed solution.
  • Step 3 providing a third solvent that is miscible with the first solvent and the second solvent, and the third solvent is obtained according to a ratio of a total of the first solvent to the second solvent to a third solvent of 1:2 to 2:1.
  • the solvent is added to the second mixed solution and uniformly mixed to obtain a quantum dot printing ink having a viscosity of 1 to 10 cps and a surface tension of 30 to 40 dyne/cm.
  • the volume ratio of the sum of the first solvent to the second solvent and the third solvent is 2:1, 1:1, or 1:2, and the like.
  • the third solvent and the second mixed solution are uniformly mixed by stirring to obtain a quantum dot printing ink.
  • the method for fabricating the quantum dot printing ink of the present invention further comprises the step of: providing a fourth solvent miscible with the first, second, and third solvents, according to the fourth solvent and the first, second, and third solvents.
  • the volume ratio of the sum is less than 1/9
  • the fourth solvent is added to the quantum dot printing ink, and the mixing is uniform
  • the viscosity of the ink for maintaining the quantum dot printing is between 1 and 10 cps
  • the surface tension is 30 to 40 dyne/cm.
  • the fourth solvent may be propylene glycol propyl ether.
  • the fourth solvent is uniformly mixed with the quantum dot printing ink by stirring.
  • the quantum dot material has a mass percentage concentration of 0.1 wt% to 10 wt%.
  • the first solvent is monoethylene glycol
  • the second solvent is 1-butanol
  • the third solvent is pyrrolidinone
  • the viscosity of the quantum dot printing ink is adjusted to a desired range by mixing the first solvent and the second solvent, and then the third solvent is mixed with the first and second solvents to maintain The viscosity of the quantum dot printing ink is adjusted to a predetermined range while adjusting the surface tension of the quantum dot printing ink.
  • the vapor pressure can be adjusted by adding a fourth solvent to the quantum dot printing ink to A reasonable range, through the mixing of the above solvents, can be formulated into a quantum dot printing ink with properties such as viscosity, surface tension and drying conditions suitable for inkjet printing, avoiding the addition of a surfactant to the ink, and obtaining the ink by inkjet printing.
  • the film does not contain a surfactant to avoid affecting the conductivity and luminescence properties of the film.
  • the present invention also provides a quantum dot printing ink comprising a quantum dot material, and a miscible first solvent, a second solvent and a third solvent, wherein the volume ratio of the first solvent to the second solvent is based on the above manufacturing method.
  • the ratio of the sum of the first solvent and the second solvent to the third solvent is 1:2 to 2:1, and the viscosity of the quantum dot printing ink is between 1 and 10 cps.
  • the surface tension is between 30 and 40 dyne/cm.
  • the quantum dot printing ink further includes a fourth solvent miscible with the first, second, and third solvents, and a volume ratio of the fourth solvent to a sum of the first, second, and third solvents is less than 1/9, the room temperature vapor of the quantum dot printing ink is pressed below 100mmHg, so that the quantum dot printing ink can be evaporated too quickly during the inkjet printing process, so that the ink droplets can be aggregated into a film to finally form a film having a uniform thickness.
  • the fourth solvent may be propylene glycol propyl ether.
  • the viscosity of the first solvent and the second solvent may not be less than 1 cps, and may not be greater than 10 cps.
  • the first solvent is monoethylene glycol; the second solvent is 1-butanol; and the third solvent is pyrrolidinone.
  • the quantum dot material has a mass percentage concentration of 0.1 wt% to 10 wt%.
  • the quantum dot material may be a nanocrystal of a group II-VI, a group III-V, a group IV element or a compound thereof.
  • the quantum dot material may be a hole injecting layer (HIL) Layer) a material, a hole transporting layer (HTL) material, an emission layer (EML) material, or an electron transporting layer (ETL) material.
  • HIL hole injecting layer
  • HTL hole transporting layer
  • EML emission layer
  • ETL electron transporting layer
  • the above quantum dot printing ink wherein the solvent is a mixed solvent containing a plurality of solvents, is a quantum dot printing ink suitable for inkjet printing, such as viscosity, surface tension, drying condition, etc., the ink does not contain a surfactant, and is printed by inkjet.
  • the film obtained from the ink does not contain a surfactant, and has good electrical conductivity and luminescent properties.
  • the present invention provides a method for fabricating a quantum dot printing ink by adjusting the viscosity of the quantum dot printing ink to a desired range by mixing the first solvent with the second solvent, and then passing the third solvent and the first 1.
  • the mixing of the second solvent adjusts the surface tension of the quantum dot printing ink to a desired range while maintaining the viscosity of the quantum dot printing ink within a predetermined range, and further, by adding the first in the quantum dot printing ink Four solvents, to adjust the vapor pressure to a reasonable range, through the mixing of the above various solvents, can formulate viscosity, surface tension, drying conditions and other performance indicators suitable for inkjet printing quantum dot printing ink, to avoid adding in the ink
  • the surfactant which is obtained by ink-jet printing the quantum dot printing ink, does not contain a surfactant, thereby avoiding influence on the conductivity and luminescent properties of the film.
  • the invention provides a quantum dot printing ink comprising a plurality of mixed solvents, which is suitable for inkjet printing quantum dot printing inks with properties such as viscosity, surface tension and drying conditions, and the ink does not contain a surfactant, and is inkjet.
  • the film obtained by printing the ink does not contain a surfactant, and has good electrical conductivity and luminescent properties.

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  • Organic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Electroluminescent Light Sources (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

提供一种量子点打印墨水的制作方法及制得的量子点打印墨水。量子点打印墨水的制作方法包括以下步骤：步骤1、提供量子点材料与第一溶剂，将量子点材料与第一溶剂混合在一起，分散均匀，得到第一混合溶液；步骤2、提供与第一溶剂互溶的第二溶剂，按照第一溶剂与第二溶剂的体积比为1:2～2:1的比例，将所述第二溶剂添加到第一混合溶液中，混合均匀，得到粘度在1～10cps之间的第二混合溶液；步骤3、提供与第一、第二溶剂互溶的第三溶剂，按照第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1的比例，将所述第三溶剂添加到第二混合溶液中，混合均匀，得到粘度在1～10cps之间，表面张力在30～40dyne/cm之间的量子点打印墨水。通过多种溶剂的混合，可以配制出粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，避免在墨水中添加表面活性剂，从而避免对薄膜的导电性及发光性能产生影响。

Description

量子点打印墨水的制作方法及制得的量子点打印墨水 技术领域
本发明涉及显示技术领域，尤其涉及一种量子点打印墨水的制作方法及制得的量子点打印墨水。
背景技术
半导体纳米晶(semiconductor nanocrystals，缩写NCs)，是指尺寸为1-100nm的半导体纳米晶粒。由于半导体纳米晶的尺寸小于其它材料的激子波尔半径，能表现出强的量子限域效应，将准连续的能带演变为类似于分子的分立能级结构，而呈现出新的材料性质，因此也称为量子点(quantum dots，缩写QDs)。
由于外部能量的激发(如光致发光、电致发光、阴极射线发光等)，电子从基态跃迁到激发态，处于激发态的电子和空穴可能会形成激子；电子与空穴发生复合，最终弛豫到基态；多余的能量通过复合和弛豫过程释放，可能辐射复合发出光子。
量子点发光二极管(Quantum Dots Light Emitting Diodes，QD-LEDs)具有重要的商业应用的价值，在最近十年引起人们强烈的研究兴趣。事实上，QD-LEDs相对于有机发光二极管(Organic Light Emitting Diodes，OLEDs)有很多的优势：(1)量子点发光的线宽在20-30nm之间，相对于有机发光>50nm的发光，半高宽(FWHM，full width at half maximum)要窄，这对于现实画面的色纯度起关键的作用；(2)无机材料相对于有机材料表现出更好的热稳定性，当器件处于高亮度或高电流密度下，焦耳热是使器件退化的主要原因，由于优异的热稳定性，基于无机材料的器件将表现出长的使用寿命；(3)由于红绿蓝三基色有机材料的寿命不同，OLEDs显示器的颜色将随时间变化，然而，用同一种材料合成不同尺寸的量子点，由于量子限域效应，可以实现三基色的发光，同一种材料可以表现出相似的退化寿命；(4)QD-LEDs可以实现红外光的发射，而有机材料的发光波长一般小于1微米；(5)对于量子点没有自旋统计的限制，其外量子效率(external quantum efficiency，EQE)有可能达到100％，QD-LED的EQE可以表示为ηExt＝ηr*ηINT*η*ηOUT，其中ηr是电子和空穴形成激子的几率，ηINT是内量子效率，即发光量子产率(PLQY)，η是辐射跃迁的几率，ηOUT是外耦合的效率。有机荧光染料ηr的限制是25％，其中单重态与三 重态的形成比例是1:3，只有单重态激子的复合导致发光，然而，由于自旋轨道耦合，有机磷光材料的ηr大于25％。值得一提的是有机磷光材料导致了母体材料的退化，平面发光器件的ηOUT大约在20％左右，可以通过微腔结构提高外耦合效率。对于QD-LEDs，其ηINT可以达到100％，当电子和空穴能级同时适合时，其ηr也可以达到100％。
喷墨印刷(ink-jet printing)是一种无接触、无压力、无印版的印刷技术，它具有无版数码印刷的共同特征，可实现各种墨水的印刷。其基本原理是将电子计算机存储的图文信息先输入到平板打印机，再通过特殊的装置，在电子计算机的控制下，由喷嘴向承印物表面喷射墨滴，墨滴铺展开来后，烘干并在需要的位置形成薄膜。
鉴于喷墨打印技术具有材料利用率高、不需要掩膜版、适合大尺寸面板制作等优点，可以将量子点材料配制成墨水，采用喷墨打印的技术进行薄膜器件制备。为了使墨水适合于喷墨打印技术，通常会对墨水的粘度和表面张力等进行调节，常用的做法是添加表面活性剂，但是当墨水干燥后，如果薄膜内残留有表面活性剂时，会对薄膜的性能产生不利的影响，表面活性剂就相当于是薄膜中的杂质，对薄膜的导电性及发光性能都会有影响。
发明内容
本发明的目的在于提供一种量子点打印墨水的制作方法，通过多种溶剂的混合，配制出粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，避免在墨水中添加表面活性剂，通过喷墨打印该量子点打印墨水得到的薄膜中不含表面活性剂，避免对薄膜的导电性及发光性能产生影响。
本发明的目的还在于提供一种量子点打印墨水，墨水中不含表面活性剂，通过喷墨打印该墨水得到的薄膜中不含表面活性剂，具有较好的导电性及发光性能。
为实现上述目的，本发明提供一种量子点打印墨水的制作方法，包括以下步骤：
步骤1、提供量子点材料与第一溶剂，将量子点材料与第一溶剂混合在一起，分散均匀，得到第一混合溶液；
步骤2、提供与第一溶剂互溶的第二溶剂，按照第一溶剂与第二溶剂的体积比为1:2～2:1的比例，将所述第二溶剂添加到第一混合溶液中，混合均匀，得到粘度在1～10cps之间的第二混合溶液；
步骤3、提供与第一、第二溶剂互溶的第三溶剂，按照第一溶剂与第二 溶剂的总和与第三溶剂的体积比为1:2～2:1的比例，将所述第三溶剂添加到第二混合溶液中，混合均匀，得到粘度在1～10cps之间，表面张力在30～40dyne/cm之间的量子点打印墨水。
还包括步骤4：提供与第一、第二、第三溶剂互溶的第四溶剂，按照第四溶剂与第一、第二、第三溶剂的总和的体积比小于1/9的比例，将第四溶剂添加到量子点打印墨水中，混合均匀，在保持量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间的同时，调节量子点打印墨水的室温蒸汽压至100mmHg以下。
所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps。
所述第一溶剂为一乙二醇；所述第二溶剂为正丁醇；所述第三溶剂为甲基吡咯烷酮；所述第四溶剂为丙二醇丙醚。
所述量子点打印墨水中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
本发明还提供一种量子点打印墨水，包括量子点材料、以及互溶的第一溶剂、第二溶剂与第三溶剂，所述第一溶剂与第二溶剂的体积比为1:2～2:1，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1，所述量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间。
还包括与第一、第二、第三溶剂互溶的第四溶剂，所述第四溶剂与所述第一、第二、第三溶剂的总和的体积比小于1/9，使得量子点打印墨水的室温蒸汽压在100mmHg以下。
所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps。
所述第一溶剂为一乙二醇；所述第二溶剂为正丁醇；所述第三溶剂为甲基吡咯烷酮；所述第四溶剂为丙二醇丙醚。
所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
本发明还提供一种量子点打印墨水，包括量子点材料、以及互溶的第一溶剂、第二溶剂与第三溶剂，所述第一溶剂与第二溶剂的体积比为1:2～2:1，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1，所述量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间；
其中，所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps；
其中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
本发明的有益效果：本发明提供的一种量子点打印墨水的制作方法，通过第一溶剂与第二溶剂的混合，将量子点打印墨水的粘度调整至一预期范围，之后通过第三溶剂与第一、第二溶剂的混合，在保持量子点打印墨水的粘度在预定范围的同时，将量子点打印墨水的表面张力调整至一预期范围，进一步的，还可以通过在量子点打印墨水中添加第四溶剂，来将其蒸汽压调节至一合理范围，通过以上多种溶剂的混合，可以配制出粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，避免在墨水中添加表面活性剂，通过喷墨打印该量子点打印墨水得到的薄膜中不含表面活性剂，避免对薄膜的导电性及发光性能产生影响。本发明提供的一种量子点打印墨水，包含多种混合的溶剂，为粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，墨水中不含表面活性剂，通过喷墨打印该墨水得到的薄膜中不含表面活性剂，具有较好的导电性及发光性能。
附图说明
为了能更进一步了解本发明的特征以及技术内容，请参阅以下有关本发明的详细说明与附图，然而附图仅提供参考与说明用，并非用来对本发明加以限制。
附图中，
图1为本发明的量子点打印墨水的制作方法的流程图。
具体实施方式
为更进一步阐述本发明所采取的技术手段及其效果，以下结合本发明的优选实施例进行详细描述。
请参阅图1，本发明提供一种量子点打印墨水的制作方法，包括以下步骤：
步骤1、提供量子点材料与第一溶剂，将量子点材料与第一溶剂混合在一起，分散均匀，得到第一混合溶液。
具体的，所述量子点材料可以是Ⅱ-Ⅵ族、Ⅲ-Ⅴ族、Ⅳ族元素或其化合物的纳米晶体。
进一步的，所述量子点材料可以是空穴注入层(hole injecting layer,HIL层)材料、空穴传输层(hole transporting layer，HTL)材料、发光层(emission layer，EML)材料、或者电子传输层(electron transporting layer，ETL)材 料。
具体的，所述步骤1中采用搅拌并超声波震荡的方式将量子点材料在第一溶剂中分散均匀，得到第一混合溶液。
步骤2、提供与第一溶剂互溶的第二溶剂，按照第一溶剂与第二溶剂的体积比为1:2～2:1的比例，将所述第二溶剂添加到第一混合溶液中，混合均匀，得到粘度在1～10cps之间的第二混合溶液。
具体的，所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps。通过调整第一溶剂与第二溶剂的体积配比，调节第二混合溶液的粘度至1～10cps之间。
优选的，所述第一溶剂与第二溶剂的体积比为2:1，1:1，或1:2等。
具体的，所述步骤2采用搅拌的方式将第二溶剂与第一混合溶液混合均匀，得到第二混合溶液。
步骤3、提供与第一、第二溶剂互溶的第三溶剂，按照第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1的比例，将所述第三溶剂添加到第二混合溶液中，混合均匀，得到粘度在1～10cps之间，表面张力在30～40dyne/cm之间的量子点打印墨水。
优选的，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为2:1，1:1，或1:2等。
通过调整第三溶剂与第一、第二溶剂的混合物的体积配比，在保持量子点打印墨水的粘度在1～10cps之间的同时，调节量子点打印墨水的表面张力至30～40dyne/cm之间。
具体的，所述步骤3采用搅拌的方式将第三溶剂与第二混合溶液混合均匀，得到量子点打印墨水。
优选的，本发明的量子点打印墨水的制作方法还包括步骤4：提供与第一、第二、第三溶剂互溶的第四溶剂，按照第四溶剂与第一、第二、第三溶剂的总和的体积比小于1/9的比例，将第四溶剂添加到到量子点打印墨水中，混合均匀，在保持量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间的同时，调节量子点打印墨水的室温蒸汽压至100mmHg以下，避免量子点打印墨水在喷墨打印的过程中蒸发过快，使得墨水滴可以汇聚成膜，最终形成厚度均匀的薄膜。
具体的，所述第四溶剂可以是丙二醇丙醚(propylene glycol propyl ether)。
具体的，所述步骤4采用搅拌的方式将第四溶剂与量子点打印墨水混合均匀。
具体的，本发明制得的量子点打印墨水中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
优选的，所述第一溶剂为一乙二醇(monoethylene glycol)；所述第二溶剂为正丁醇(1-butanol)；所述第三溶剂为甲基吡咯烷酮(pyrrolidinone)。
上述量子点打印墨水的制作方法，通过第一溶剂与第二溶剂的混合，将量子点打印墨水的粘度调整至一预期范围，之后通过第三溶剂与第一、第二溶剂的混合，在保持量子点打印墨水的粘度在预定范围的同时，将量子点打印墨水的表面张力调整至一预期范围，进一步的，还可以通过在量子点打印墨水中添加第四溶剂，来将其蒸汽压调节至一合理范围，通过以上溶剂的混合，可以配制出粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，避免在墨水中添加表面活性剂，通过喷墨打印该墨水得到的薄膜中不含表面活性剂，避免对薄膜的导电性及发光性能产生影响。
基于上述制作方法，本发明还提供一种量子点打印墨水，包括量子点材料、以及互溶的第一溶剂、第二溶剂与第三溶剂，其中，所述第一溶剂与第二溶剂的体积比为1:2～2:1，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1，所述量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间。
进一步的，所述量子点打印墨水还包括与第一、第二、第三溶剂互溶的第四溶剂，所述第四溶剂与所述第一、第二、第三溶剂的总和的体积比小于1/9，使得量子点打印墨水的室温蒸汽压在100mmHg以下，避免量子点打印墨水在喷墨打印的过程中蒸发过快，使得墨水滴可以汇聚成膜，最终形成厚度均匀的薄膜。
具体的，所述第四溶剂可以是丙二醇丙醚(propylene glycol propyl ether)。
具体的，所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps。优选的，所述第一溶剂为一乙二醇(monoethylene glycol)；所述第二溶剂为正丁醇(1-butanol)；所述第三溶剂为甲基吡咯烷酮(pyrrolidinone)。
具体的，所述量子点打印墨水中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
具体的，所述量子点材料可以是Ⅱ-Ⅵ族、Ⅲ-Ⅴ族、Ⅳ族元素或其化合物的纳米晶体。
进一步的，所述量子点材料可以是空穴注入层(hole injecting layer,HIL 层)材料、空穴传输层(hole transporting layer，HTL)材料、发光层(emission layer，EML)材料、或者电子传输层(electron transporting layer，ETL)材料。
上述量子点打印墨水，其溶剂为包含多种溶剂的混合溶剂，为粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，墨水中不含表面活性剂，通过喷墨打印该墨水得到的薄膜中不含表面活性剂，具有较好的导电性及发光性能。
综上所述，本发明提供的一种量子点打印墨水的制作方法，通过第一溶剂与第二溶剂的混合，将量子点打印墨水的粘度调整至一预期范围，之后通过第三溶剂与第一、第二溶剂的混合，在保持量子点打印墨水的粘度在预定范围的同时，将量子点打印墨水的表面张力调整至一预期范围，进一步的，还可以通过在量子点打印墨水中添加第四溶剂，来将其蒸汽压调节至一合理范围，通过以上多种溶剂的混合，可以配制出粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，避免在墨水中添加表面活性剂，通过喷墨打印该量子点打印墨水得到的薄膜中不含表面活性剂，避免对薄膜的导电性及发光性能产生影响。本发明提供的一种量子点打印墨水，包含多种混合的溶剂，为粘度、表面张力、干燥条件等性能指标适合喷墨打印的量子点打印墨水，墨水中不含表面活性剂，通过喷墨打印该墨水得到的薄膜中不含表面活性剂，具有较好的导电性及发光性能。
以上所述，对于本领域的普通技术人员来说，可以根据本发明的技术方案和技术构思作出其他各种相应的改变和变形，而所有这些改变和变形都应属于本发明权利要求的保护范围。

Claims (13)

  1. 一种量子点打印墨水的制作方法，包括以下步骤：
    步骤1、提供量子点材料与第一溶剂，将量子点材料与第一溶剂混合在一起，分散均匀，得到第一混合溶液；
    步骤2、提供与第一溶剂互溶的第二溶剂，按照第一溶剂与第二溶剂的体积比为1:2～2:1的比例，将所述第二溶剂添加到第一混合溶液中，混合均匀，得到粘度在1～10cps之间的第二混合溶液；
    步骤3、提供与第一、第二溶剂互溶的第三溶剂，按照第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1的比例，将所述第三溶剂添加到第二混合溶液中，混合均匀，得到粘度在1～10cps之间，表面张力在30～40dyne/cm之间的量子点打印墨水。
  2. 如权利要求1所述的量子点打印墨水的制作方法，还包括步骤4：提供与第一、第二、第三溶剂互溶的第四溶剂，按照第四溶剂与第一、第二、第三溶剂的总和的体积比小于1/9的比例，将第四溶剂添加到量子点打印墨水中，混合均匀，在保持量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间的同时，调节量子点打印墨水的室温蒸汽压至100mmHg以下。
  3. 如权利要求1所述的量子点打印墨水的制作方法，其中，所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps。
  4. 如权利要求2所述的量子点打印墨水的制作方法，其中，所述第一溶剂为一乙二醇；所述第二溶剂为正丁醇；所述第三溶剂为甲基吡咯烷酮；所述第四溶剂为丙二醇丙醚。
  5. 如权利要求1所述的量子点打印墨水的制作方法，其中，所述量子点打印墨水中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
  6. 一种量子点打印墨水，包括量子点材料、以及互溶的第一溶剂、第二溶剂与第三溶剂，所述第一溶剂与第二溶剂的体积比为1:2～2:1，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1，所述量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间。
  7. 如权利要求6所述的量子点打印墨水，还包括与第一、第二、第三溶剂互溶的第四溶剂，所述第四溶剂与所述第一、第二、第三溶剂的总和的体积比小于1/9，使得量子点打印墨水的室温蒸汽压在100mmHg以下。
  8. 如权利要求6所述的量子点打印墨水，其中，所述第一溶剂与第二 溶剂的粘度不能都小于1cps，也不能都大于10cps。
  9. 如权利要求7所述的量子点打印墨水，其中，所述第一溶剂为一乙二醇；所述第二溶剂为正丁醇；所述第三溶剂为甲基吡咯烷酮；所述第四溶剂为丙二醇丙醚。
  10. 如权利要求6所述的量子点打印墨水，其中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
  11. 一种量子点打印墨水，包括量子点材料、以及互溶的第一溶剂、第二溶剂与第三溶剂，所述第一溶剂与第二溶剂的体积比为1:2～2:1，所述第一溶剂与第二溶剂的总和与第三溶剂的体积比为1:2～2:1，所述量子点打印墨水的粘度在1～10cps之间，表面张力在30～40dyne/cm之间；
    其中，所述第一溶剂与第二溶剂的粘度不能都小于1cps，也不能都大于10cps；
    其中，所述量子点材料的质量百分比浓度为0.1wt％～10wt％。
  12. 如权利要求11所述的量子点打印墨水，还包括与第一、第二、第三溶剂互溶的第四溶剂，所述第四溶剂与所述第一、第二、第三溶剂的总和的体积比小于1/9，使得量子点打印墨水的室温蒸汽压在100mmHg以下。
  13. 如权利要求11所述的量子点打印墨水，其中，所述第一溶剂为一乙二醇；所述第二溶剂为正丁醇；所述第三溶剂为甲基吡咯烷酮；所述第四溶剂为丙二醇丙醚。
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