CN115851038A - Ternary solvent-based red quantum dot ink-jet ink and preparation method thereof - Google Patents
Ternary solvent-based red quantum dot ink-jet ink and preparation method thereof Download PDFInfo
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- 238000007641 inkjet printing Methods 0.000 claims abstract description 17
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- UJMBCHVRTIOTKC-UHFFFAOYSA-N cyclobutylbenzene Chemical compound C1CCC1C1=CC=CC=C1 UJMBCHVRTIOTKC-UHFFFAOYSA-N 0.000 claims description 2
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- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 2
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- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
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- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to the field of ink-jet printing, and also relates to red quantum dot ink-jet ink based on a ternary solvent and a preparation method thereof. The ink comprises the following components in parts by weight: the solvent consists of a quantum dot material, a medium-boiling point solvent and a high-boiling point solvent, and specifically comprises the following components in volume ratio: 50.0-60.0% of medium boiling point solvent, 6.7-33.3% of first high boiling point solvent and 33.3-60.0% of second high boiling point solvent; the boiling point range of the medium boiling point solvent is 100-200 ℃, the boiling point range of the high boiling point solvent is 200-300 ℃, and the boiling point of the high boiling point solvent is higher than that of the medium boiling point solvent; the vapor pressure of the medium-boiling point solvent of the solvent is 1.0kPa to 1.5kPa, the vapor pressure of the first high-boiling point solvent is 0kPa to 0.5kPa: the vapor pressure of the first high-boiling point solvent is 0.5kPa to 1.0kPa. According to the technical scheme, the generation of coffee rings can be further inhibited, and the uniformity of film formation can be improved.
Description
Technical Field
The invention belongs to the technical field of ink-jet printing, and relates to red quantum dot ink-jet ink based on a ternary solvent and a preparation method thereof.
Background
In recent years, with the continuous improvement of the preparation method of the QLED (quantum dot light emitting diode), the QLED material is rapidly developed in the aspect of display screen application. In the field of luminescent display applications, ink jet printing has been a significant manufacturing technique in printing manufacture that is not negligible. Compared with the traditional evaporation method and spin-coating method, the method has the advantages that the QLED is prepared more simply and conveniently by using the ink-jet printing process technology, the utilization rate of materials is improved, and the method is more favorable for achieving the aims of large area, high color gamut, high efficiency, low cost, industrialization and the like of the QLED in display application.
With the continuous updating of luminescent materials, the QLED has gradually exhibited a trend exceeding LCD and OLED in display preparation and application due to its characteristics of high luminous efficiency, stable optical performance, long luminous life, and the like, and the QLED display screen will be available in the future in the field of luminescent display application.
In the aspect of QLED display application, the prepared quantum dot ink, the charge transmission conductive ink and the electrode material can be sprayed to a set area of a printed substrate through a nozzle by using an ink-jet printing technology, and after the preparation of each functional layer of a QLED device is finished, the preparation of the QLED light-emitting device is finished. Although the inkjet printing technology will become the mainstream way of preparing the QLED, continuous adjustment and improvement are needed in the inkjet printing process to solve the matching problem with the quantum dot ink.
The formulation of the ink and the adjustment of the ink-jet printing process will affect the stability of ink-jet printing and the uniformity of the quantum dot film. In the actual preparation process, the coffee ring phenomenon easily occurs on the quantum dot film, and the occurrence of the coffee ring influences the light-emitting uniformity of the QLED. The impact of different solvents on the performance of quantum dot materials should therefore be explored in the formulation of inks, while controlling the relevant parameters of inkjet printing technology to avoid the coffee ring effect.
In the prior art, most researches on inhibition of coffee rings are based on preparation of quantum dot ink of a unitary solvent or a binary solvent, and various flatting agents, surfactants and the like are added after an organic solvent is added to improve the uniformity of a film and inhibit the coffee rings. However, the above technical solutions in the prior art still have the appearance of coffee rings on the one hand and the film forming effect on the other hand, which are mainly reflected in that the uniformity and roughness of the film forming are not ideal enough.
Disclosure of Invention
The invention provides a pure solvent type red quantum dot ink-jet ink based on a ternary solvent and a preparation method thereof, and aims to solve the technical problem that a quantum dot film is prepared based on ink-jet printing.
In order to solve the above technical problems, the technical solution provided by the present invention includes:
the red quantum dot ink-jet ink based on the ternary solvent is mainly used for ink-jet printing, and is characterized by comprising a solvent, wherein the solvent consists of a quantum dot material, a medium-boiling point solvent and a high-boiling point solvent, and specifically comprises the following components in volume ratio: 50.0-60.0% of medium boiling point solvent, 6.7-33.3% of first high boiling point solvent and 33.3-60.0% of second high boiling point solvent; the boiling point range of the medium boiling point solvent is 100-200 ℃, the boiling point range of the high boiling point solvent is 200-300 ℃, and the boiling point of the high boiling point solvent is higher than that of the medium boiling point solvent; the vapor pressure of the medium-boiling point solvent of the solvent is 1.0kPa to 1.5kPa, the vapor pressure of the first high-boiling point solvent is 0kPa to 0.5kPa: the vapor pressure of the first high-boiling point solvent is 0.5kPa to 1.0kPa. And the quantum dot material accounts for 1-8% of the ink by weight.
Preferably, the medium-boiling point solvent is at least one of alkane, alkene and aromatic hydrocarbon; the high boiling point solvents are all selected from at least one of alkane, alkene, aromatic hydrocarbon, alcohol, ester and ether.
Preferably, the ternary solvent-based red quantum dot inkjet ink consists of an organic solvent and a quantum dot material, and does not include other materials.
Preferably, the solvent used comprises at least one of n-methane, n-ethane, n-propane, n-butane, n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane, n-undecane, n-dodecane, n-tridecane, n-tetradecane, n-pentadecane, n-hexadecane, n-heptadecane, n-octadecane, n-nonadecane, n-eicosane, n-triacontane, n-forty-alkylcyclopropane, cyclobutane, cyclopentane, cyclohexane, 1-undecene, 1-dodecene, 1-octadecene, phenylcyclopropane, phenylcyclobutane, phenylcyclopentane, phenylcyclohexane, 1,2-propanediol, 1,3-propanediol, cycloethanol, cyclopropanol, cyclohexanol, benzyl alcohol, butyl benzoate, isobornyl acrylate, neopentyl glycol diacrylate, isobornyl methacrylate, 3,4 dimethyl anisole, p-diphenyl ether.
Preferably, the quantum dot material is a powdery red quantum dot material, the particle size is 10-15nm, and the luminous efficiency is more than 85%.
A method of preparing a red quantum dot inkjet ink for inkjet printing as described in any one of the above, comprising the steps of: (1) Fully stirring and mixing the two high-boiling-point solvents, stirring by using an electric stirrer at a stirring speed of 330 r/min-800 r/min for 5-20 min, and uniformly mixing to obtain a component A; (2) Fully stirring and mixing the component A and a medium-boiling point solvent at the stirring speed of 330-800 r/min for 5-20 min to obtain a component B; (3) And (2) fully stirring and mixing the quantum dot material and the component B according to the formula of the ink, uniformly stirring by using an electric stirrer at the stirring speed of 330-800 r/min for 5-20 min, and preparing to obtain the ink.
The three solvents used by the pure solvent type red quantum dot ink-jet ink based on the ternary solvent have different boiling points and different vapor pressures. Most of the traditional quantum dot printing ink is binary solvent, in the evaporation process, because the vapor pressure of the solvent is different, the solvent with higher vapor pressure can be volatilized firstly, only one solvent is left to continue to finish the evaporation process, at the moment, because only one organic solvent participates in evaporation, and the coffee ring phenomenon can not uniformly appear on the film after the evaporation and drying are finished. The quantum dot ink-jet ink using the ternary solvent is based on the principle of solvent evaporation, introduces an organic solvent with intermediate vapor pressure, and after the high-vapor-pressure solvent is volatilized, two solvents with different vapor pressures are left to participate in the evaporation process, so that the stability of the evaporation process is ensured, and the phenomenon of coffee ring caused by the instability of the evaporation process due to the overlarge vapor pressure difference of the binary solvent is avoided.
Therefore, the technical scheme can inhibit the coffee ring effect of the quantum dot film and avoid the phenomenon of uneven luminous performance of the follow-up quantum dot light-emitting diode. Moreover, the uniformity of the film is improved, and the roughness of the quantum dot film is reduced. In addition, the ink in the technical scheme of the invention is pure solvent type quantum dot ink, and only three organic solvents with different boiling points, viscosities, vapor pressures and surface tensions are used for uniformly dispersing the quantum dot material, so that the influence of other additives on the performance of the quantum dot material can be avoided, and the stable performance of the quantum dot material can be maintained. The preparation cost of the quantum dot ink is reduced while the addition of various materials such as a leveling agent, a surfactant and the like is reduced.
In the invention, the solvents selected by the quantum dot ink are weak polar solvents or nonpolar solvents, which is beneficial to the uniform dispersion and long-term stable storage of quantum dot materials. The 'ternary' in the quantum dot ink points to the amount of the solvent selected in the preparation of the quantum dot ink, and the solvent defined as a medium boiling point is used as a good solvent of a quantum dot material in the quantum dot ink to play a role in dissolving the quantum dot material; for solvents defined as high boiling points, the surface tension of the quantum dot ink is primarily adjusted, and the drying rate of the quantum dot ink is also controlled. During ink jet printing, quantum dot ink needs to be filtered firstly, and then the diameter of a nozzle of ink jet printing needs to be selected to prevent the nozzle from being blocked. The surface of the ink-jet printed quantum dot film is uniform, and the roughness is reduced; the pure organic solvent is selected in the formula of the printing ink to uniformly disperse the quantum dot material, so that the influence of other additives on the quantum dot material, the whole rheological property of the printing ink and the light emitting property of a quantum dot light emitting diode device can be avoided, and meanwhile, the time cost, the manufacturing process cost and the material cost are also reduced.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, various changes or modifications of the present invention may be made by those skilled in the art, and equivalents may fall within the scope of the claims of the present application. In terms of volume ratio.
In the specific embodiment, the quantum dot material CdSe/CdS/ZnS is a powdery red quantum dot material with the particle size of 10-15nm and the luminous efficiency>85 percent and the density of the mixture is between 0.8 and 1.0g/cm -3 (25 ℃), viscosity is less than 2cP (25 ℃), and surface tension is 26-28 mN/m (25 ℃); solvents selected by the quantum dot ink are weak polar solvents or nonpolar solvents.
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 9:1) were mixed, placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane =9: 1).
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 8:2) were mixed, placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane =8: 2), placing the mixture in a magnetic stirrer for stirring for 5 minutes, finally mixing the quantum dot material with a volume fraction of 4% with the mixed solvent containing the three solvents, and stirring the mixture in the magnetic stirrer for 15 minutes to obtain the uniform quantum dot ink.
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 7:3) were mixed, placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane =7: 5), placing the mixture in a magnetic stirrer, stirring for 5 minutes, finally mixing the quantum dot material with the volume fraction of 5% with the mixed solvent containing the three solvents, and stirring for 15 minutes in the magnetic stirrer to obtain the uniform quantum dot ink.
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 6:4) were mixed, placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane =6: 5), placing the mixture in a magnetic stirrer, stirring for 5 minutes, finally mixing the quantum dot material with the volume fraction of 6% with the mixed solvent containing the three solvents, and stirring for 15 minutes in the magnetic stirrer to obtain the uniform quantum dot ink.
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 5:5) were mixed, placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane = 5).
[ example 6 ]
Two high boiling solvents (cyclohexylbenzene: butyl benzoate = 7:3) were mixed and placed in a magnetic stirrer and stirred for 5 minutes to stir well. And mixing n-octane with a high-boiling-point mixed solvent (cyclohexylbenzene: butyl benzoate: n-octane =7: 6), placing the mixture in a magnetic stirrer, stirring for 5 minutes, finally mixing the quantum dot material with the volume fraction of 9% with the mixed solvent of the three solvents, and stirring for 15 minutes in the magnetic stirrer to obtain the uniform quantum dot ink.
The properties of the quantum dot inks prepared in examples 1-6 are shown in Table 1. The density of the red quantum dot ink-jet ink is 0.8-1.0 g/cm -3 (25 ℃), viscosity is less than 2cP (25 ℃), surface tension is 26-28 mN/m (25 ℃), and jetting Z value is large but can meet the requirement of ink-jet printing under the adjustment of ink-jet voltage and waveform.
TABLE 1 Properties of inks prepared in examples 1-6
Note: both viscosity and surface tension were tested in an environment at 25 ℃.
The quantum dot inks prepared in examples 1-6 were dried completely on both the outside and the inside.
Claims (6)
1. A red quantum dot ink-jet ink based on a ternary solvent, which is mainly used for ink-jet printing, is characterized in that the ink-jet ink comprises,
the solvent consists of a quantum dot material, a medium-boiling point solvent and a high-boiling point solvent, and specifically comprises the following components in volume ratio: 50.0-60.0% of medium boiling point solvent, 6.7-33.3% of first high boiling point solvent and 33.3-60.0% of second high boiling point solvent; the boiling point range of the medium boiling point solvent is 100-200 ℃, the boiling point range of the high boiling point solvent is 200-300 ℃, and the boiling point of the high boiling point solvent is higher than that of the medium boiling point solvent; the vapor pressure of the medium-boiling point solvent of the solvent is 1.0kPa to 1.5kPa, the vapor pressure of the first high-boiling point solvent is 0kPa to 0.5kPa: the vapor pressure of the first high boiling point solvent is 0.5 kPa-1.0 kPa;
and
the ink comprises a quantum dot material, wherein the quantum dot material accounts for 1-8% of the ink by weight.
2. The ternary solvent-based red quantum dot inkjet ink according to claim 1,
the medium boiling point solvent is at least one of alkane, olefin and aromatic hydrocarbon; the high boiling point solvents are all selected from at least one of alkane, alkene, aromatic hydrocarbon, alcohol, ester and ether.
3. The ternary solvent based red quantum dot inkjet ink according to claim 1, wherein: the ternary solvent-based red quantum dot inkjet ink is composed of an organic solvent and a quantum dot material, and does not include other materials.
4. The ternary solvent based red quantum dot inkjet ink according to claim 1, wherein: the solvent used includes at least one of n-methane, n-ethane, n-propane, n-butane, n-pentane, n-hexane, n-heptane, n-octane, n-nonane, n-decane, n-undecane, n-dodecane, n-tridecane, n-tetradecane, n-pentadecane, n-hexadecane, n-heptadecane, n-octadecane, n-nonadecane, n-eicosane, n-triacontane, n-forty-alkylcyclopropane, cyclobutane, cyclopentane, cyclohexane, 1-undecene, 1-dodecene, 1-octadecene, phenylcyclopropane, phenylcyclobutane, phenylcyclopentane, phenylcyclohexane, 1,2-propanediol, 1,3-propanediol, cycloethanol, cyclopropanol, cyclohexanol, benzyl alcohol, butyl benzoate, isobornyl acrylate, neopentyl glycol diacrylate, isobornyl methacrylate, 3,4 dimethyl anisole, p-diphenyl ether 3956.
5. The ternary solvent based red quantum dot inkjet ink according to claim 1, wherein the quantum dot material is a powdered red quantum dot material, the particle size is 10-15nm, and the luminous efficiency is >85%.
6. The method of preparing the ternary solvent based red quantum dot inkjet ink as claimed in any one of claims 1 to 4, comprising the steps of:
(1) Fully stirring and mixing the two high-boiling-point solvents, stirring by using an electric stirrer at a stirring speed of 330 r/min-800 r/min for 5-20 min, and uniformly mixing to obtain a component A;
(2) Fully stirring and mixing the component A and a medium-boiling point solvent at the stirring speed of 330-800 r/min for 5-20 min to obtain a component B;
(3) And (2) fully stirring and mixing the quantum dot material and the component B according to the formula of the ink, uniformly stirring by using an electric stirrer at the stirring speed of 330-800 r/min for 5-20 min, and preparing to obtain the ink.
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