CN112442300B - Preparation method of quantum dot ink and quantum dot light-emitting diode - Google Patents
Preparation method of quantum dot ink and quantum dot light-emitting diode Download PDFInfo
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Abstract
The invention belongs to the technical field of display, and particularly relates to a preparation method of quantum dot ink and a quantum dot light-emitting diode. A quantum dot ink includes a solvent including a non-polar solvent and a polar solvent miscible with the non-polar solvent, and quantum dots dispersed in the solvent. The polar solvent can be mutually soluble with a main solvent, namely a non-polar solvent, in the quantum dot ink, and the film forming property of the quantum dot ink can be improved by adding the polar solvent, namely, the repulsion between interfaces is reduced when the quantum dot ink is printed on the surface of a functional layer of a QLED device, and the interface contact angle is reduced, so that the orderliness of a contact surface crystal between a quantum dot light-emitting layer and the functional layer is optimized, the quantum dot light-emitting layer is uniformly spread, and the film forming property of a device film layer is optimized.
Description
Technical Field
The invention belongs to the technical field of display, and particularly relates to a preparation method of quantum dot ink and a quantum dot light-emitting diode.
Background
Quantum dots have the advantages of high color purity, wide color gamut, adjustable Light Emitting wavelength, solubility, and the like, and Quantum Dot Light Emitting Diodes (QLEDs) are considered as one of the most promising materials for the development of technology. Among them, the inkjet printing of quantum dots is a solution processing technology with high efficiency and low cost, and the technology has high material utilization rate and simple process, and is considered as an effective way to solve the cost problem and realize a large-area display panel. The ink-jet printing technology can accurately deposit quantum dots and other transmission layer materials at pixel positions by using ink, the quantum dots and the transmission layer materials need ink with different polarities so as to achieve an orthogonal effect, and the ink has great influence on the luminous performance of a QLED device, so that the preparation of the ink is a great problem in quantum dot printing.
Inevitably, quantum dots need to be printed on the transmission layer, the quantum dot ink with weaker polarity forms a mutually exclusive interface on the surface of the transmission layer material with the hydrophilicity, the film forming property and interface contact of the quantum dot ink are influenced, the problems of poor uniformity, high roughness and the like of a quantum dot film layer are caused, the leakage current phenomenon occurs on partial sites, the problems of uneven light emission, black dots and the like of a QLED device are caused, and the light emitting performance of the device is greatly influenced.
Disclosure of Invention
The invention aims to provide a quantum dot ink and a preparation method of a quantum dot light-emitting diode, and aims to solve the technical problem of poor film forming uniformity of quantum dots in the conventional quantum dot light-emitting diode.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides quantum dot ink which comprises a solvent and quantum dots dispersed in the solvent, wherein the solvent comprises a non-polar solvent and a polar solvent mutually soluble with the non-polar solvent.
The quantum dot ink provided by the invention is added with a polar solvent which plays a role of interface buffering in the solvent as an auxiliary solvent, the polar solvent can be mutually dissolved with a main solvent, namely a non-polar solvent, in the quantum dot ink, and the film forming property of the quantum dot ink can be improved by adding the polar solvent, so that the repulsion force between interfaces can be reduced when the quantum dot ink is printed on the surface of a functional layer of a QLED device, and the interface contact angle is reduced, thereby optimizing the ordering of crystals on a contact surface between a quantum dot light-emitting layer and the functional layer, uniformly spreading the quantum dot light-emitting layer, optimizing the film forming property of a device film layer, finally avoiding the defect that the local over thickness of the quantum dot light-emitting layer causes the overhigh lighting voltage or the local over-thinness of the quantum dot light-emitting layer causes the leakage current, and improving the overall light-emitting uniformity.
The invention provides a preparation method of a quantum dot light-emitting diode, which comprises the following steps:
providing a substrate, wherein a functional layer is arranged on the surface of the substrate;
the quantum dot ink is printed on the surface of the functional layer, and then drying treatment is carried out to obtain the quantum dot light-emitting layer.
The preparation method of the quantum dot light-emitting diode provided by the invention is characterized in that the specific quantum dot ink is printed into the quantum dot light-emitting layer, and a polar solvent playing a role in interface buffering in the solvent is added into the quantum dot ink to serve as an auxiliary solvent, so that when the quantum dot ink is printed on the surface of the functional layer of the QLED device, the repulsion force between interfaces is reduced, the interface contact angle is reduced, the ordering of crystals on the contact surface between the quantum dot light-emitting layer and the functional layer is optimized, the quantum dot light-emitting layer is uniformly spread, and finally the defect of leakage current caused by overhigh lighting voltage or overlow local quantum dot light-emitting layer due to over-thick local quantum dot light-emitting layer can be avoided, and the overall light-emitting performance of the device is improved.
Drawings
Fig. 1 is a schematic flow chart of a method for manufacturing a quantum dot light-emitting diode according to an embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In one aspect, an embodiment of the present invention provides a quantum dot ink, including a solvent and quantum dots dispersed in the solvent, where the solvent includes a non-polar solvent and a polar solvent miscible with the non-polar solvent.
In the quantum dot ink provided by the embodiment of the invention, a polar solvent playing an interface buffering role in a solvent is added as an auxiliary solvent, the polar solvent can be mutually soluble with a main solvent, namely a non-polar solvent, in the quantum dot ink, and the film forming property of the quantum dot ink can be improved by adding the polar solvent, namely, when the quantum dot ink is printed on the surface of a functional layer of a QLED device, the repulsion force between interfaces is reduced, and the interface contact angle is reduced, so that the ordering of crystals at the contact surface between a quantum dot light-emitting layer and the functional layer is optimized, the quantum dot light-emitting layer is uniformly spread, the film forming property of a device film layer is optimized, the defect that the lighting voltage is too high due to the local over-thickness of the quantum dot light-emitting layer or the leakage current is caused by the local over-thickness of the quantum dot light-emitting layer is finally avoided, and the overall light-emitting uniformity is improved.
In one embodiment, the volume ratio of the non-polar solvent to the polar solvent is (95:5) - (99.5: 0.5). Namely, the polar solvent accounts for 0.5 to 5.0 percent of the total volume of the solvent of the quantum dot ink; if the proportion is too low, the interface buffer effect cannot be achieved in the solvent, and the contact angle between the quantum dot ink and the functional layer (such as an electron transport layer or a hole transport layer) is slightly influenced; if the proportion is too high, the solubility of the quantum dots in the ink is affected, and the problems of turbidity, even precipitation and the like occur. Therefore, the polar solvent in the above range is not only well soluble in the main solvent, i.e., the nonpolar solvent, but also has little influence on the solubility of the quantum dot in the ink.
In one embodiment, the concentration of quantum dots in the quantum dot ink is 1-200 mg/mL. More preferably 10-30mg/mL, and within this concentration range, the printing performance and film-forming performance of the quantum dot ink are better. In the embodiment of the present invention, the quantum dot in the quantum dot ink may be an oily quantum dot, and the surface of the quantum dot may be connected with a ligand that is easily soluble in a solvent with a relatively low polarity, for example, the ligand on the surface of the quantum dot includes at least one of an acid ligand, a thiol ligand, an amine ligand, an (oxy) phosphine ligand, a phospholipid ligand, a lecithin ligand, a polyvinylpyridine ligand, and the like. As a specific embodiment, the acid ligand is at least one of deca acid, undecylenic acid, tetradecanoic acid, oleic acid and stearic acid; the mercaptan ligand is at least one of octaalkylmercaptan, dodecyl mercaptan and octadecyl mercaptan; the amine ligand comprises at least one of oleylamine, octadecylamine and octaamine; the (oxy) phosphine ligand is at least one of trioctylphosphine and trioctylphosphine. The material of the quantum dot may be at least one of group II-IV semiconductor compounds, group III-V semiconductor compounds, group IV-VI semiconductor compounds, and group I-II-VI2 semiconductor nanocrystals. Specifically, the II-IV group semiconductor compound includes but is not limited to at least one of CdS, CdSe, CdS/ZnS, CdSe/CdS/ZnS; the III-V semiconductor compound and the IV-VI semiconductor compound include but are not limited to at least one of GaAs, InP, PbS/ZnS and PbSe/ZnS. In the quantum dot ink, the concentration of the quantum dots is 1-200mg/mL, preferably 10-30mg/mL, and within the concentration range, the printing performance and the film-forming performance of the quantum dot ink are relatively good.
In one embodiment, the non-polar solvent has a boiling point of 150-330 ℃; if the boiling point of the non-solvent is too low, the uniformity problems of coffee rings and other film-forming can occur during film-forming; if the boiling point is too high, the ink cannot be completely volatilized in the ink jet printing equipment, and the performance of the device is influenced. In another embodiment, the surface tension of the non-polar solvent is 20-40mN/m, the viscosity of the non-polar solvent is 1-10 cP; if the surface tension or viscosity of the nonpolar solvent is too low, the flowability of the solvent is too high, and the film-forming problems such as coffee rings and the like are easily formed; too high a surface tension or viscosity will result in too high a contact angle, again affecting film formation.
In one embodiment, the polar solvent has a boiling point of 140-340 ℃. Specifically, the polar solvent and the non-polar solvent have boiling points that differ by no more than 50 ℃. The difference between the boiling point of the polar buffer solvent and the boiling point of the main solvent is not more than 50 ℃, and the two solvents can keep similar volatilization rates during film forming so as to ensure the uniformity of film forming.
In one embodiment, the non-polar solvent is selected from at least one of an alkane solvent, an alkene solvent, and an aromatic solvent; the polar solvent is at least one selected from ester solvents, ether solvents and ketone solvents. Specifically, the non-polar solvent is a saturated hydrocarbon and/or non-saturated hydrocarbon solvent containing 6 to 18 carbon atoms, preferably a saturated hydrocarbon and/or non-saturated hydrocarbon solvent containing 6 to 18 carbon atoms, which has a surface tension of 20 to 40mN/m and a viscosity in the range of 1 to 10 cP; the polar solvent is at least one of an ester solvent containing 6-18 carbon atoms, an ether solvent containing 6-18 carbon atoms and a ketone solvent containing 6-18 carbon atoms. In a specific embodiment, the alkane solvent in the nonpolar solvent is selected from at least one of tetradecane, n-hexane, n-heptane, n-octane, cyclohexane, cycloheptane, and cyclooctane; the olefinic solvent in the nonpolar solvent is at least one selected from the group consisting of 1-decene, 1-dodecene, 1-tetradecene, and 1-hexadecene; the aromatic hydrocarbon solvent in the nonpolar solvent is at least one selected from the group consisting of benzene, toluene and xylene. And the ester solvent in the polar solvent is at least one selected from the group consisting of n-pentyl butyrate, n-hexyl propionate and n-heptyl butyrate; at least one of n-hexyl ether, n-heptyl ether and n-octane which are the ether solvents in the polar solvent; the ketone solvent in the polar solvent is at least one of 2-hexanone, 2-heptanone and 2-octanone.
On the other hand, the embodiment of the invention also provides a preparation method of the quantum dot light emitting diode, as shown in fig. 1, the preparation method comprises the following steps:
s01: providing a substrate, wherein a functional layer is arranged on the surface of the substrate;
s02: the quantum dot ink is printed on the surface of the functional layer, and then drying treatment is carried out to obtain the quantum dot light-emitting layer.
According to the preparation method of the quantum dot light-emitting diode provided by the embodiment of the invention, the specific quantum dot ink provided by the embodiment of the invention is printed into the quantum dot light-emitting layer, and the polar solvent which plays a role in interface buffering in the solvent is added into the quantum dot ink to serve as the auxiliary solvent, so that when the quantum dot ink is printed on the surface of the functional layer of the QLED device, the repulsion between interfaces is reduced, and the interface contact angle is reduced, thereby optimizing the ordering of the crystal of the contact surface between the quantum dot light-emitting layer and the functional layer, uniformly spreading the quantum dot light-emitting layer, and finally avoiding the defect of leakage current caused by overhigh lighting voltage or overlow local quantum dot light-emitting layer due to overhigh local thickness of the quantum dot light-emitting layer, so that the overall light-emitting performance of the device is improved.
The functional layer is a transport layer, and the specific material may be an electron transport layer material (which may be an organic or inorganic electron transport layer material), or a hole transport layer material, which may be TFB, PVK, nickel oxide, zinc oxide, or the like.
In one embodiment, the structure of the quantum dot light emitting diode may include, from bottom to top, a cathode, an electron transport layer, a quantum dot light emitting layer, a hole transport layer, and an anode. Therefore, the substrate is a cathode substrate, and the functional layer is an electron transport layer; the quantum dot ink is directly printed on the surface of the electron transport layer, and then drying treatment is carried out to obtain the quantum dot light-emitting layer.
In another embodiment, the structure of the quantum dot light emitting diode may include, from bottom to top, an anode, a hole transport layer, a quantum dot light emitting layer, an electron transport layer, and a cathode. Thus, the substrate is an anode substrate and the functional layer is a hole transport layer; thus, the quantum dot ink is directly printed on the surface of the hole transport layer, and then drying treatment is carried out to obtain the quantum dot light-emitting layer.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
The quantum dot ink provided in this embodiment is a green CdSe quantum dot, the concentration of the quantum dot in the ink is 40mg/mL, the main solvent, that is, the nonpolar solvent is tetradecane, and the polar buffer solvent is n-hexyl ether, where the proportion of tetradecane in the solvent is 98.0%, and the proportion of n-hexyl ether is 2.0%.
A QLED device comprises an anode, a hole transport layer, a quantum dot light-emitting layer, an electron transport layer and a cathode which are stacked; the quantum dot light-emitting layer is prepared by printing the quantum dot ink on a hole transport layer or an electron transport layer.
In the QLED device, the electron transport layer is zinc oxide, the hole transport layer is TFB, after 2.0% of n-hexyl ether is added into the quantum dot ink, compared with the quantum dot ink with 100% of tetradecane serving as a solvent, the contact angle of the quantum dot ink of the embodiment with the zinc oxide electron transport layer is reduced by 2 degrees, the contact angle of the quantum dot ink with the TFB hole transport layer is reduced by 4 degrees, the film forming property is improved, and the light-emitting quantum yield is 24.7%.
Example 2
The embodiment provides a quantum dot ink, wherein quantum dots in the quantum dot ink are red CdSe quantum dots, the concentration of the red CdSe quantum dots in the ink is 40mg/mL, a main solvent, namely a nonpolar solvent is cyclooctane, and a polar buffer solvent is 2-octanone, wherein the proportion of tetradecane in the solvent is 98.0%, and the proportion of 2-octanone is 2.0%.
A QLED device comprises an anode, a hole transport layer, a quantum dot light-emitting layer, an electron transport layer and a cathode which are stacked; the quantum dot light-emitting layer is prepared by printing the quantum dot ink on a hole transport layer or an electron transport layer.
In the QLED device, the electron transport layer is zinc oxide, the hole transport layer is PVK, and after 2.0% of 2-octanone is added to the quantum dot ink, compared with the quantum dot ink in which the solvent is 100% of cyclooctane, the contact angle of the quantum dot ink of the present embodiment with the zinc oxide electron transport layer is reduced by 2 degrees, the contact angle with the PVK hole transport layer is reduced by 2 degrees, the film forming property is improved, and the luminescent quantum yield is 19.2%.
Example 3
The embodiment provides quantum dot ink, wherein quantum dots in the quantum dot ink are blue light CdS quantum dots, the concentration of the quantum dots in the ink is 40mg/mL, a main solvent, namely a nonpolar solvent is 1-tetradecene, a polar buffer solvent is n-amyl butyrate, the proportion of tetradecane in the solvent is 98.0%, and the proportion of n-amyl butyrate is 2.0%
A QLED device comprises an anode, a hole transport layer, a quantum dot light-emitting layer, an electron transport layer and a cathode which are stacked; the quantum dot light-emitting layer is prepared by printing the quantum dot ink on a hole transport layer or an electron transport layer.
In the QLED device, the electron transport layer is made of zirconium oxide, the hole transport layer is made of nickel oxide, after 2.0% of n-amyl butyrate is added into the quantum dot ink, compared with the quantum dot ink with the solvent 100% of 1-tetradecene, the contact angle of the quantum dot ink of the embodiment with the zirconium oxide electron transport layer is reduced by 3 degrees, the contact angle with the nickel oxide hole transport layer is reduced by 5 degrees, the film forming property is improved, and the luminous quantum yield is 21.3%.
Example 4
A preparation method of a QLED device comprises the following steps:
a: firstly, printing a hole transport layer on an ITO substrate, wherein the hole transport layer is made of TFB ink, and heating, vacuumizing and drying the hole transport layer;
b: printing quantum dot ink on the hole transport layer, wherein the quantum dot is CdS @ ZnS blue quantum dot wrapped with oleylamine ligand, the main solvent of the ink is 98.0% of 1-tetradecene, and the polar buffer solvent is 2.0% of n-amyl butyrate, and then heating, vacuumizing and drying;
c: and finally, printing an electronic transmission layer on the quantum dot light-emitting layer, and evaporating a cathode on the electronic transmission layer to obtain the QLED.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. The quantum dot ink is composed of a solvent and quantum dots dispersed in the solvent, and is characterized in that the solvent comprises a non-polar solvent and a polar solvent mutually soluble with the non-polar solvent, and the volume ratio of the non-polar solvent to the polar solvent is (95:5) - (99.5: 0.5);
the difference between the boiling points of the polar solvent and the nonpolar solvent is not more than 50 ℃, the viscosity of the nonpolar solvent is 1-10cP, the surface tension of the nonpolar solvent is 20-40mN/m, the nonpolar solvent is selected from an olefin solvent, and the polar solvent is selected from at least one of an ester solvent and an ether solvent.
2. The quantum dot ink of claim 1, wherein the concentration of quantum dots in the quantum dot ink is 1-200 mg/mL.
3. The quantum dot ink as claimed in claim 1, wherein the non-polar solvent has a boiling point of 150-330 ℃; and/or the presence of a gas in the gas,
the boiling point of the polar solvent is 140-340 ℃.
4. The quantum dot ink of any one of claims 1-3, wherein the olefinic solvent is selected from at least one of 1-decene, 1-dodecene, 1-tetradecene, and 1-hexadecene; and/or the presence of a gas in the gas,
the ester solvent is at least one of n-amyl butyrate, n-hexyl propionate and n-heptyl butyrate; and/or the presence of a gas in the gas,
the ether solvent is at least one selected from n-hexyl ether and n-heptyl ether.
5. The quantum dot ink according to any one of claims 1 to 3, wherein the non-polar solvent is an olefinic solvent having 6 to 18 carbon atoms; and/or the presence of a gas in the gas,
the polar solvent is at least one of an ester solvent containing 6-18 carbon atoms and an ether solvent containing 6-18 carbon atoms.
6. A preparation method of a quantum dot light-emitting diode is characterized by comprising the following steps:
providing a substrate, wherein a functional layer is arranged on the surface of the substrate;
printing the quantum dot ink as claimed in any one of claims 1 to 5 on the surface of the functional layer, and then carrying out drying treatment to obtain the quantum dot light-emitting layer.
7. The method according to claim 6, wherein the substrate is a cathode substrate, and the functional layer is an electron transport layer; or, the substrate is an anode substrate, and the functional layer is a hole transport layer.
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| CN105820662A (en) * | 2016-04-26 | 2016-08-03 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
| CN108659616A (en) * | 2017-03-27 | 2018-10-16 | Tcl集团股份有限公司 | A kind of printing ink of inkjet printing and preparation method thereof |
| CN109181414A (en) * | 2017-07-14 | 2019-01-11 | 苏州星烁纳米科技有限公司 | quantum dot ink and light emitting diode |
| CN110085749A (en) * | 2018-06-15 | 2019-08-02 | 广东聚华印刷显示技术有限公司 | Quantum dot ink and preparation method thereof and quantum dot light emitting device |
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| ES2342189T3 (en) * | 2006-12-21 | 2010-07-02 | Agfa Graphics N.V. | PRINTING METHOD BY INK JET AND INK CARTRIDGES. |
| CN105153807B (en) * | 2015-07-21 | 2016-10-19 | 京东方科技集团股份有限公司 | Quantum dot ink |
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| CN105820662A (en) * | 2016-04-26 | 2016-08-03 | Tcl集团股份有限公司 | Quantum dot ink and preparation method thereof |
| CN108659616A (en) * | 2017-03-27 | 2018-10-16 | Tcl集团股份有限公司 | A kind of printing ink of inkjet printing and preparation method thereof |
| CN109181414A (en) * | 2017-07-14 | 2019-01-11 | 苏州星烁纳米科技有限公司 | quantum dot ink and light emitting diode |
| CN110085749A (en) * | 2018-06-15 | 2019-08-02 | 广东聚华印刷显示技术有限公司 | Quantum dot ink and preparation method thereof and quantum dot light emitting device |
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