WO2012098578A1 - 有機発光素子の製造方法、有機表示パネル、有機発光装置、機能層の形成方法、インク、基板、有機発光素子、有機表示装置、および、インクジェット装置 - Google Patents
有機発光素子の製造方法、有機表示パネル、有機発光装置、機能層の形成方法、インク、基板、有機発光素子、有機表示装置、および、インクジェット装置 Download PDFInfo
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- WO2012098578A1 WO2012098578A1 PCT/JP2011/000256 JP2011000256W WO2012098578A1 WO 2012098578 A1 WO2012098578 A1 WO 2012098578A1 JP 2011000256 W JP2011000256 W JP 2011000256W WO 2012098578 A1 WO2012098578 A1 WO 2012098578A1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/145—Arrangement thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/17—Ink jet characterised by ink handling
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2202/00—Embodiments of or processes related to ink-jet or thermal heads
- B41J2202/01—Embodiments of or processes related to ink-jet heads
- B41J2202/09—Ink jet technology used for manufacturing optical filters
Definitions
- the present invention relates to a method for manufacturing an organic light emitting element, an organic display panel, an organic light emitting device, a method for forming a functional layer, an ink, a substrate, an organic light emitting element, an organic display device, and an ink jet device.
- Organic light-emitting devices that have been researched and developed in recent years are light-emitting devices that utilize the electroluminescence phenomenon of functional materials, and an organic light-emitting layer composed of a functional material is interposed between an anode and a cathode. Has a structured.
- a functional material including an organic light emitting layer is formed by vapor-depositing a functional material on a substrate by a vapor deposition method using a mask.
- a coating method is proposed separately from the vapor deposition method (Patent Document 1).
- a functional material is dissolved in a solvent to form an ink, and the ink is ejected from an ink ejection nozzle of an ink jet apparatus to apply the ink onto the substrate.
- the process does not need to be performed in a vacuum vessel, and a mask is not required, which is preferable in terms of mass production.
- an ink is accurately applied to a light emitting layer forming region on a substrate to form an organic light emitting layer having a uniform film thickness and shape.
- the flying characteristics of the ink droplets ejected from the ink jet apparatus must be suitable, that is, the ink droplets must have a characteristic of reaching the target position without being split straight. .
- the flying characteristics of ink droplets are easily affected by ink physical properties such as ink density, ink surface tension, ink viscosity, and ink droplet diameter, and the relationship between these ink physical properties is unknown. It is not easy to control the flight characteristics. In addition, the flight characteristics change depending on factors other than ink physical properties, such as the ink droplet diameter, which is mainly determined by the nozzle diameter of the ink discharge nozzle, and the discharge speed of the ink droplets discharged from the ink discharge nozzle. Is not easy.
- the present invention can easily and accurately infer conditions that provide suitable flight characteristics. Therefore, an organic light-emitting element that can efficiently produce an organic light-emitting element having good light-emitting characteristics by a coating method.
- the main purpose is to provide a manufacturing method.
- a method for manufacturing an organic light-emitting device includes a functional material constituting a functional layer and having a weight average molecular weight of greater than 0 and 100000 or less, and the functional material.
- a fourth step of drying the droplets to form the functional layer; and a fifth step of forming a second electrode above the functional layer, and the density of the ink in the first step (g / m 3), the surface tension ⁇ (mN ⁇ m) and the viscosity ⁇ (mPa ⁇ s), and nozzle diameter r of the ink ejection nozzle (mm) is, Z (Ohnesorge number Oh below Equation 1]
- the ink droplet ejection speed V (m / s) in the third step satisfies the numerical range of the following [Equation 2], and the Z value and the ejection speed V ( m / s) is set so as to satisfy the following relational expression [Equation 3].
- An organic light-emitting device manufacturing method includes an ink density ⁇ (g / m 3 ), a surface tension ⁇ (mN ⁇ m), a viscosity ⁇ (mPa ⁇ s), and a nozzle of an ink discharge nozzle.
- the diameter r (mm) satisfies the numerical range of the Z value of the above [Equation 1] (the reciprocal of the Ohnesorge number Oh), and the ink droplet ejection speed V (m / s) is the numerical range of the above [Equation 2].
- the Z value and the discharge speed V (m / s) are set so as to satisfy the relational expression [Formula 3].
- the Z value and the discharge speed V (m Since only two of / s) are used, it is easy to guess the change in flight characteristics. Further, since the Z value and the discharge speed V (m / s) are highly correlated with the flight characteristics, accurate estimation is possible. Therefore, conditions for achieving suitable flight characteristics can be estimated easily and accurately, and an organic light-emitting element having good light-emitting characteristics can be efficiently manufactured by a coating method.
- 1 is a diagram illustrating a schematic configuration of an ink jet apparatus according to an aspect of the present invention. It is process drawing for demonstrating the manufacturing method of the organic light emitting element which concerns on 1 aspect of this invention. It is process drawing for demonstrating the manufacturing method of the organic light emitting element which concerns on 1 aspect of this invention.
- 1 is a perspective view illustrating an organic display device and the like according to one embodiment of the present invention.
- 1 is a diagram illustrating an entire configuration of a display device according to one embodiment of the present invention. It is a figure which shows the organic light-emitting device which concerns on 1 aspect of this invention.
- An organic light-emitting device manufacturing method includes a functional material that forms a functional layer and has a weight average molecular weight of greater than 0 and less than or equal to 100,000, and a solvent that dissolves the functional material.
- a first step of filling the ink jet apparatus with an ink discharge nozzle with the ink, a second step of preparing a substrate on which a base layer including a first electrode is formed, and the ink jet device to the substrate A third step of disposing the ink droplets as ink droplets from the ink jet apparatus and landing the ink droplets on the base layer of the substrate; drying the ink droplets; A fourth step of forming a layer, a fifth step of forming a second electrode above the functional layer,
- the density ⁇ (g / m 3 ), the surface tension ⁇ (mN ⁇ m) and the viscosity ⁇ (mPa ⁇ s) of the ink, and the nozzle diameter r (mm) of the ink discharge nozzle ) Satisfies the numerical range of Z in [Equation 1] (the reciprocal of Ohnesorge number Oh), and the ejection speed V (m / s) of the ink droplet in the third step is the numerical value in [
- the value of Z is 2 or more and 10 or less, and the discharge speed V is 3 (m / s) or more and 5 (m / s).
- the density ⁇ of the ink is greater than 827 (g / m 3 ) and 1190 (g / m 3 ) or less.
- the surface tension ⁇ is greater than 27.3 (mN ⁇ m) and 41.9 (mN ⁇ m) or less, and the viscosity ⁇ of the ink is greater than 2.4 (mPa ⁇ s) and 35.0 (mPa ⁇ s). S) or less, and the nozzle diameter r of the ink jet apparatus is 0.02 (mm) or more and 0.03 (mm) or less.
- the second step includes an opening corresponding to the pixel portion, and a plurality of partition walls that divide adjacent pixel portions above the base layer.
- the ink droplets are landed on the base layer facing the opening between the partition walls of the substrate.
- the organic display panel according to one embodiment of the present invention uses an organic light-emitting element manufactured by the method for manufacturing an organic light-emitting element.
- An organic light-emitting device manufactured by the method for manufacturing an organic light-emitting element was used for the organic light-emitting device according to one embodiment of the present invention.
- An organic display device uses an organic light-emitting element manufactured by the method for manufacturing an organic light-emitting element.
- the method for forming a functional layer according to one embodiment of the present invention includes an ink that forms a functional layer and includes a functional material having a weight average molecular weight of greater than 0 and less than or equal to 100,000 and a solvent that dissolves the functional material.
- the density ⁇ (g / m 3 ), the surface tension ⁇ (mN ⁇ m) and the viscosity ⁇ (mPa ⁇ s) of the ink, and the nozzle diameter r ( m m) satisfies the numerical range of Z in [Equation 1] (the reciprocal of the Ohnesorge number Oh), and the ejection speed V (m / s) of the ink droplet in the third step is as expressed in [Equation 2].
- the numerical value range is satisfied, and the value of Z and the discharge speed V (m /
- the value of Z is 2 or more and 10 or less, and the discharge speed V is 3 (m / s) or more and 5 (m / s). It is as follows.
- the density ⁇ of the ink is greater than 827 (g / m 3 ) and equal to or less than 1190 (g / m 3 ), and the surface of the ink
- the tension ⁇ is greater than 27.3 (mN ⁇ m) and 41.9 (mN ⁇ m) or less
- the viscosity ⁇ of the ink is greater than 2.4 (mPa ⁇ s) and 35.0 (mPa ⁇ s). s) or less
- the nozzle diameter r of the inkjet device is 0.02 (mm) or more and 0.03 (mm) or less.
- An ink according to an aspect of the present invention is an ink for forming a functional layer that is ejected using an ink jet apparatus including an ink ejection nozzle and is landed on a substrate and dried to form the functional layer.
- a functional material having a weight average molecular weight of greater than 0 and less than or equal to 100,000 and a solvent that dissolves the functional material, the density ⁇ (g / m 3 ), the surface tension ⁇ (mN ⁇ m ) And its viscosity ⁇ (mPa ⁇ s), and the nozzle diameter r (mm) of the ink discharge nozzle satisfy the numerical range of Z (the reciprocal number of the Ohnesorge number Oh) in the above [Equation 1].
- the ink is discharged at a discharge speed V (m / s) that satisfies the numerical range of [Expression 2], and the value of Z satisfies the relational expression of [Expression 3] with respect to the discharge speed V (m / s). .
- the organic light-emitting element substrate including the functional material constituting the functional layer of the organic light-emitting element and the solvent in the organic light-emitting element substrate including the functional material constituting the functional layer of the organic light-emitting element and the solvent, and the base layer including the first electrode is formed. And an ink for forming a functional layer of the organic light emitting element between the first electrode and the second electrode facing the base layer, which is landed on the base layer and dried.
- the density ⁇ (g / m 3 ), the surface tension ⁇ (mN ⁇ m), and the viscosity ⁇ (mPa ⁇ s) are determined by the discharge speed V.
- the Z value is set to satisfy 2 to 10 inclusive.
- the density ⁇ is 827 (g / m 3).
- the surface tension ⁇ is greater than 27.3 (mN ⁇ m) and 41.9 (mN ⁇ m) or less, and the viscosity ⁇ is 2. It is larger than 4 (mPa ⁇ s) and not more than 35.0 (mPa ⁇ s).
- the substrate according to one embodiment of the present invention has a functional layer manufactured using the above ink.
- the organic light emitting device has a functional layer manufactured using the above ink.
- An organic display panel includes an organic light-emitting element having a functional layer manufactured using the above ink.
- An organic light-emitting device includes an organic light-emitting element having a functional layer manufactured using the above ink.
- An organic display device includes an organic light-emitting element having a functional layer manufactured using the above ink.
- An ink jet device contains an ink including a functional material that constitutes a functional layer and has a weight average molecular weight of greater than 0 and less than or equal to 100,000, and a solvent that dissolves the functional material,
- An ink jet apparatus for forming a functional layer by discharging the ink from an ink discharge nozzle and landing on a substrate, wherein the nozzle diameter r (mm) of the ink discharge nozzle is a density ⁇ (g / g of the ink).
- the functional material of the ink is a functional material constituting a functional layer of an organic light emitting element, and the ink is ejected and the ink is used as the first electrode.
- the functional layer of the organic light-emitting device is landed on the base layer of the organic light-emitting element substrate on which the base layer containing the organic light-emitting element is formed, and between the first electrode and the second electrode facing the base layer. Inkjet device for forming.
- the substrate according to one embodiment of the present invention has a functional layer manufactured using the above-described inkjet device.
- the organic light-emitting element according to one embodiment of the present invention includes a functional layer manufactured using the above-described inkjet device.
- An organic display panel includes an organic light-emitting element that has a functional layer and is manufactured using the inkjet device.
- An organic light-emitting device includes an organic light-emitting element that has a functional layer and is manufactured using the inkjet device.
- An organic display device includes an organic light-emitting element having a functional layer, which is formed using the above-described inkjet device.
- FIG. 1 is a diagram for explaining three forces that affect the flying characteristics of ink droplets. As shown in FIG. 1, the flying characteristics of ink droplets are determined by the balance of three forces: viscous resistance, inertial force, and surface tension.
- the viscous resistance is determined by the ink viscosity ⁇ , the ink droplet diameter r ′, and the ejection speed V as shown in [Formula 1] below.
- Viscous force ⁇ ⁇ r ⁇ v ... [Formula 1]
- the inertial force is determined by the ink density ⁇ , the ink droplet diameter r ′, and the ejection speed V as shown in [Formula 2] below.
- Inertia force ⁇ ⁇ r 2 ⁇ v 2 [Formula 2]
- the surface tension is determined by the ink surface tension ⁇ and the ink droplet diameter r ′ as shown in [Formula 3] below.
- ink density ⁇ ink density ⁇
- ink surface tension ⁇ ink viscosity ⁇
- ink droplet diameter r ′ the four factors of ink density ⁇ , ink surface tension ⁇ , ink viscosity ⁇ , and ink droplet diameter r ′ are factors related to ink physical properties, and only the discharge speed V is a factor other than ink physical properties. is there. If all of these factors are variables, there are as many as five variables, and their mutual relations are unknown, so it is very difficult to control the flight characteristics.
- the Reynolds number Nre is a dimensionless number defined by the ratio of inertia force and viscous force, and is a value used for examining the property of “flow” in fluid mechanics. In the present application, it is considered to be mainly involved in the straightness of the ink droplet.
- the Reynolds number Nre is expressed as a ratio of inertial force to viscous force as shown in [Expression 4] below.
- Weber number Nwe is a dimensionless number that is important when dealing with two-phase flow. It is a value used for organizing deformation behavior when droplets flow in an air stream and stability problems at the interface of droplets. is there. In the present application, it is considered to be mainly involved in the splitting property of ink droplets.
- the Weber number Nwe is represented by the ratio between the inertial force and the surface tension, as shown in [Formula 5] below.
- the inventors have come up with the idea that the flight characteristics are controlled by two variables: the Z value, which is a factor related to ink physical properties, and the ejection speed V, which is a factor other than ink physical properties. Therefore, it was decided to confirm the correlation between the Z value and the flight characteristics and the correlation between the discharge speed V and the flight characteristics, respectively. Since the Z value and the discharge speed V are independent values, the correlation between the Z value and the flight characteristics, and the correlation between the discharge speed V and the flight characteristics, were intended to be determined separately.
- the straightness of the ink droplets must be good. Good straightness means that the ink droplets ejected from the ink jet apparatus reach the target position straightly. Straightness can be evaluated by measuring the landing accuracy of ink droplets, for example.
- FIG. 2 is a diagram for explaining the landing accuracy of ink droplets. The landing accuracy of ink droplets will be described with reference to FIG.
- an ink jet head When applying ink by an application method using an ink jet apparatus, generally, an ink jet head is disposed above a substrate, and ink droplets are discharged downward from an ink discharge nozzle.
- the distance between the substrate and the inkjet head at this time is, for example, about 500 ( ⁇ m).
- the substrate has a plurality of banks (partition walls) partitioning the light emitting layer formation region (pixel portion) on the upper surface.
- the light emitting layer forming region has a width of about 60 ( ⁇ m), for example, and the bank has a width of about 30 ( ⁇ m) and a thickness of about 1 ( ⁇ m), for example.
- the ink ejection nozzle has, for example, a nozzle diameter r (diameter) of about 20 ( ⁇ m), and the ink droplet ejected therefrom has an ink droplet diameter r ′ of about 24 ( ⁇ m).
- the ink droplet is ejected with an error of ⁇ 10 ( ⁇ m) or less. Is preferred. From the above, when the error is ⁇ 10 ( ⁇ m) or less, that is, when the landing accuracy is 20 ( ⁇ m) or less, it is determined that the straightness is good.
- FIG. 3 is a diagram showing experimental results on the relationship between the Z value and the landing accuracy.
- Functional materials and solvents constituting the ink ink concentration (concentration of the functional material with respect to ink), ink viscosity ⁇ , ink surface tension ⁇ and ink density ⁇ , and nozzle discharge nozzle diameter r as shown in the table
- the Z value was controlled by changing, and ink droplets were ejected under the conditions described with reference to FIG. 2, and the landing accuracy was measured and evaluated with a standard deviation of 6 ⁇ . Since the ink droplet diameter r ′ depends on the nozzle diameter r of the ink discharge nozzle, the nozzle diameter r is used in place of the ink droplet diameter r ′.
- the experiment was conducted in order to obtain an evaluation of an ink using a functional material having a weight average molecular weight of greater than 0 and less than 100000 (in the figure of the present application, abbreviated as “100k”). This was carried out with an ink using a functional material having an average molecular weight of 100,000. Furthermore, as an alternative to an ink composed of a functional material having a weight average molecular weight as close to 0 as possible, an ink composed of a functional material having a weight average molecular weight of 0, that is, an ink containing no functional material (solvent alone )
- solvent A is 1-nonanol
- solvent B is dimethyl phthalate
- solvent K represents cyclohexylbenzene.
- FIG. 4 is a diagram showing the relationship between the Z value and the landing accuracy.
- the experimental data No. 1 shown in FIG. 3 is shown on the XY coordinates where the Z value is taken on the X axis and the landing accuracy is taken on the Y axis.
- 1 to No. 20 are plotted, it can be seen that there is a correlation between the Z value and the satellite generation rate. It can also be seen that the smaller the Z value, the worse the landing accuracy, and when the Z value is less than 0.7, the landing accuracy exceeds 20 ( ⁇ m). From the above, the lower limit of the Z value was set to 0.7. Further, as apparent from the slope of the approximate curve shown in FIG. 4, it is considered that the Z value is preferably 2 or more from the viewpoint of good and stable landing accuracy.
- the reason why the landing accuracy is deteriorated when the Z value is small is considered to be that, for example, when the ink viscosity ⁇ is high, the ink droplets from the ink discharge nozzles are poorly cut, so that the ligament becomes long and the landing accuracy deteriorates. It is done. On the other hand, when the ink viscosity ⁇ is low, the ink droplets are cut well, so the ligament is shortened and the landing accuracy is improved.
- FIG. 5 is a diagram showing the relationship between the discharge speed V and the landing accuracy. As a result of the measurement, results as shown in FIG. 5 were obtained. Accordingly, it was found that there is a correlation between the discharge speed V and the landing accuracy, and the landing accuracy is good when the discharge speed V is equal to or higher than a predetermined speed. This is presumably because the ink droplets are more likely to flow into the air stream as the discharge speed V is lower, and it is difficult for the ink droplets to flow into the air stream when the discharge speed V is higher. It has been found that if the discharge speed V is 3 (m / s) or more, the landing accuracy will not exceed the allowable limit of 20 ( ⁇ m) even if some errors are taken into consideration. 3 (m / s).
- FIG. 6 is a diagram showing the relationship between the discharge speed V and the discharge speed variation.
- the discharge speed V is taken on the X axis, and the value obtained by dividing the standard deviation of the discharge speed by the average value of the discharge speed V is taken on the Y axis.
- the discharge speed V is 3 (m / s) or more and 5 (m / s) or less
- the value of the Y-axis is 2 (%) or less, and it is difficult to be affected by the airflow. Therefore, it can be said that the discharge speed V is more preferably 3 (m / s) or more and 5 (m / s) or less.
- FIG. 7 is a diagram for explaining the mode of breakup of ink droplets.
- One aspect of ink droplet splitting is when the ink droplet splits into a small number of droplets.
- the droplet is split into two droplets A and B.
- the ink droplets are split in this way, it is impossible to determine which of the small droplets is the main droplet, making it impossible to manage the discharge operation.
- the ink droplet splitting there is a case where the ink droplet splits into a main droplet and a plurality of satellites (meaning small droplets split from the main droplet).
- the main droplet C is divided into a plurality of satellites D.
- FIG. 7C In order to make it easier to visually understand the mode of ink droplet splitting, the schematic diagram of the image shown in FIG. 7A is shown in FIG. 7C, and the schematic diagram of the image shown in FIG. This is shown in FIG.
- Fissionability was evaluated by the following method.
- the splitting property was evaluated by confirming the presence or absence of splitting by observing the flight of ink droplets.
- the flight observation was performed by, for example, observing the droplet shape after ejection at a resolution of 1 (usec) using an inkjet evaluation apparatus Litrex 120L (manufactured by ULVAC, Inc.).
- the upper limit of the discharge speed V was set to 6 (m / s).
- a preferable range of the discharge speed V is 3 (m / s) or more and 6 (m / s) or less.
- the satellite generation speed is a speed at which satellites are generated when the speed is higher than that speed, and is a speed that sets an upper limit for obtaining good flight characteristics determined with respect to the Z value of each ink droplet.
- FIG. 8 is a diagram showing the relationship between the Z value and the satellite generation speed.
- FIG. 9 is a diagram showing an aspect of ink droplets in region I in FIG.
- FIG. 10 is a diagram showing an aspect of ink droplets in region II in FIG.
- FIG. 11 is a diagram showing an aspect of ink droplets in region III in FIG.
- the ink viscosity ⁇ was measured using a viscometer AR-G2 (TA Instruments).
- the ink surface tension ⁇ was measured using a surface tension meter DSA100 (manufactured by KRUSS).
- the ink density ⁇ was calculated from the specific gravity (assuming the specific gravity is 1 because the functional material has a low concentration).
- the satellite has a satellite viscosity ⁇ of about 15 (mPa ⁇ s) and the ink viscosity ⁇ of about 1 (mPa ⁇ s).
- the ink droplets were ejected one by one in a normal state.
- region II in FIG. 8 as shown in FIG. 10A, when the ink viscosity ⁇ is about 15 (mPa ⁇ s), the ligament of the ink droplet (meaning the ink tailing phenomenon) becomes long.
- the ink viscosity ⁇ was about 1 (mPa ⁇ s), it did not occur.
- FIG. 9A the schematic diagram of the image shown in FIG. 9A is shown in FIG. 9B
- FIG. 10B shows a schematic diagram of the image shown in FIG. 11A
- FIG. 11A the schematic diagram of the image shown in FIG. 11A
- the functional material and solvent constituting the ink, the ink concentration (ratio of the functional material in the ink), the ink viscosity ⁇ , the ink surface tension ⁇ , the ink density ⁇ , and the nozzle diameter r are changed at the levels shown in the table.
- the Z value was controlled, ink droplets were ejected under the conditions described with reference to FIG. 2, and the ejection speed V at which satellites were generated was measured. Since the ink droplet diameter r ′ depends on the nozzle diameter r of the ink discharge nozzle, the nozzle diameter r is used in place of the ink droplet diameter r ′.
- the experiment was conducted in order to obtain an evaluation of an ink using a functional material having a weight average molecular weight of greater than 0 and less than or equal to 100,000, and an ink using a functional material having a weight average molecular weight of 100,000 and a weight average molecular weight of 0. This was performed with an ink using the functional material (ink containing no functional material).
- FIG. 12 is a diagram showing experimental results regarding the relationship between the Z value and the satellite generation speed.
- the Z value of 21 was 15.0, satellites were generated when the discharge speed V was 2.7 (m / s) or higher.
- No. When the Z value of 22 was 33.8, satellites were generated when the discharge speed V was 0.9 (m / s) or more.
- the discharge speed V is 3.0 (m / s) or more.
- the satellite generation rate is 2.7 (m / s). In No. 21, when the discharge speed V is set to 2.7 (m / s) or more, satellites are generated. That is, no. In 21, it is impossible to make both straightness and splitting good. Therefore, no. 21 determined the splitting ability to be “x”. Similarly, all of the satellites having a satellite generation rate of 3.0 (m / s) or less were determined to be “ ⁇ ”. On the other hand, if the satellite generation rate exceeds 3.0 (m / s), good splitting ability may be obtained.
- solvent a is acetophenone
- solvent b is xylene
- solvent l is methoxytoluene
- solvent m is cyclohexylbenzene.
- FIG. 13 is a diagram showing the relationship between the Z value and the satellite generation speed.
- the experimental data No As shown in FIG. 13, on the XY coordinates where the Z value is taken on the X axis and the satellite generation speed is taken on the Y axis, the experimental data No.
- a regression equation as shown in [Equation 8] below was obtained, and it was found that there was a correlation between the Z value and the satellite generation rate. Therefore, it is possible to estimate the speed at which satellites are generated from the Z value.
- the splitting property of the ink droplet does not depend only on the ejection velocity V but depends on both the ejection velocity V and the Z value. It has been found that it is important that the Z value and the discharge speed V satisfy a predetermined relationship in order to improve the quality.
- the present invention was reached by investigating that there was an unexpected correlation between the Z value and the discharge speed V, which were assumed to be independently defined at the beginning of the study. I was able to.
- FIG. 14 is a diagram summarizing the relationship between the Z value, the satellite generation speed (FIG. 13), and the landing accuracy (FIG. 4).
- the area indicated by hatching in the graph shown in FIG. 14 is an area where the landing accuracy is good and no satellite is generated with respect to the Z value, that is, an area where good flight characteristics are obtained. If the Z value is increased by increasing the ink viscosity or the like, the splitting property is improved (meaning that it is difficult to split), but the straightness is deteriorated. On the other hand, if the Z value is decreased, the splitting property is deteriorated (meaning that it is easy to split), but the straightness is improved.
- the inventors have demonstrated that the flying characteristics of ink droplets can be controlled by the Z value, and have demonstrated through experiments that there is a correlation between the flying characteristics of ink droplets and the Z value. That is, it is used by generalizing the relationship between the ink viscosity Z, the surface tension ⁇ and density ⁇ , and the Z value of the ink droplet determined by the nozzle diameter r of the ink ejection nozzle, and the flying characteristics of the ink droplet. According to the inkjet head to be used, it was possible to predict the ink physical properties that would give good flight characteristics, and succeeded in controlling the flight characteristics of the ink droplets. This makes it possible to reduce the burden of ink development and ejection evaluation.
- the discharge speed V it is possible to more accurately grasp the relationship with the flight characteristics.
- the inventors obtained an aspect that suitable flight characteristics can be obtained by controlling the Z value and the discharge speed V so as to satisfy the above [Equation 1] to [Equation 3].
- the Z value is 2 or more and 10 or less, more suitable flight characteristics can be obtained.
- An ink according to an embodiment of the present invention includes a functional material that forms a functional layer and a solvent that dissolves the functional material, and is suitable for an ink physical property suitable for an ink jet method (droplet discharge method) using an ink jet apparatus.
- the ink density ⁇ is larger than 827 (g / m 3 ) and 1190 (g / m 3 ) or less, and the ink surface tension ⁇ is 27.3 (as shown in FIG. 3 and FIG.
- the nozzle diameter r of the ink discharge nozzle of the ink jet apparatus is preferably 0.02 (mm) or more and 0.03 (mm) or less.
- F8-F6 (a copolymer of F8 (polydioctylfluorene) and F6 (polydihexylfluorene)) is preferable as the functional material.
- fluorene compounds other than F8-F6 such as F8 and F6, oxinoid compounds, perylene compounds, coumarin compounds, azacoumarin compounds, oxazole compounds, oxadiazole compounds, perinone compounds, pyrrolopyrrole compounds, naphthalene compounds, Anthracene compound, fluoranthene compound, tetracene compound, pyrene compound, coronene compound, quinolone compound and azaquinolone compound, pyrazoline derivative and pyrazolone derivative, rhodamine compound, chrysene compound, phenanthrene compound, cyclopentadiene compound, stilbene compound, diphenylquinone compound, styryl compound
- the above-described experiment regarding the correlation between the Z value and the flight characteristics and the correlation between the ejection speed V and the flight characteristics is performed using a functional material having a weight average molecular weight of greater than 0 and less than or equal to 100,000.
- a functional material having a weight average molecular weight of greater than 0 and less than or equal to 100,000 is suitable, for example, for an ink for forming a light emitting functional layer that emits red light or green light.
- the thickness of the green light emitting functional layer is, for example, 60 to 100 (nm).
- the weight average molecular weight is greater than 0 and less than or equal to 100,000. It is preferable to use the functional material.
- a functional material having a weight average molecular weight of 80,000 or more and 100,000 or less is more preferable.
- the functional material is F8-F6, the minimum value of the weight average molecular weight is theoretically 722.
- FIG. 15 is a diagram showing the relationship between the Z value, ink density, and ink viscosity ⁇ .
- the Z value, ink density, and ink viscosity ⁇ shown in FIG. 15 are values when F8-F6 is used as the functional material and a mixed solvent of cyclohexylbenzene and methoxytoluene (mixing ratio 8: 2) is used as the solvent. .
- the ink concentration (wt / vol) is preferably in the range of 0.5 (%) to 3.0 (%), and the ink viscosity ⁇ is 4
- the preferred range is from 0.5 (mPa ⁇ s) to 28.0 (mPa ⁇ s), and the Z value is from 0.9 to 6.0.
- the solvent when the functional material is F8-F6, cyclohexylbenzene, methoxytoluene, methylnaphthalene, xylene and the like are suitable.
- the solvent only needs to dissolve the functional material, and may be a single solvent or a mixture of a plurality of solvents.
- FIG. 16 is a schematic diagram illustrating a stacked state of each layer of the organic display panel according to one embodiment of the present invention.
- an organic display panel 110 according to one embodiment of the present invention has a structure in which a color filter substrate 113 is bonded to the organic light-emitting element 111 according to one embodiment of the present invention with a sealant 112 interposed therebetween. .
- the organic light emitting element 111 is a top emission type organic light emitting element in which RGB pixels are arranged in a matrix or a line, and each pixel has a stacked structure in which each layer is stacked on the TFT substrate 1.
- the first anode electrode 2 and the second anode electrode 3 constituting the first electrode are formed in a matrix shape or a line shape, and a hole injection layer 4 is laminated on the anode electrodes 2 and 3. Furthermore, a bank 5 for defining pixels is formed on the hole injection layer 4.
- a substrate 11 according to one embodiment of the present invention includes a TFT substrate 1, anode electrodes 2 and 3, and a bank 5, and includes a plurality of banks 5 including openings 12 corresponding to the pixel portions and partitioning adjacent pixel portions. Is formed above the anode electrodes 2 and 3.
- a hole transport layer 6 and an organic light emitting layer 7 are laminated in this order in the region defined by the bank 5. Further, on the organic light emitting layer 7, an electron transport layer 8, a cathode electrode 9 as a second electrode, and a sealing layer 10 are connected to the adjacent pixels beyond the area defined by the bank 5. It is formed to do.
- the region defined by the bank 5 has a multilayer laminated structure in which a hole injection layer 4, a hole transport layer 6, an organic light emitting layer (functional layer) 7, and an electron transport layer 8 are laminated in that order.
- Typical configurations of the multilayer structure are (1) hole injection layer / organic light emitting layer, (2) hole injection layer / hole transport layer / organic light emitting layer, and (3) hole injection layer / organic light emitting layer / electron injection.
- Layer (4) hole injection layer / hole transport layer / organic light emitting layer / electron injection layer, (5) hole injection layer / organic light emitting layer / hole blocking layer / electron injection layer, (6) hole injection layer / hole transport layer / Organic light emitting layer / hole blocking layer / electron injection layer, (7) organic light emitting layer / hole blocking layer / electron injection layer, and (8) organic light emitting layer / electron injection layer.
- the TFT substrate 1 is, for example, alkali-free glass, soda glass, non-fluorescent glass, phosphoric acid glass, boric acid glass, quartz, acrylic resin, styrene resin, polycarbonate resin, epoxy resin, polyethylene, polyester, silicone type.
- An amorphous TFT (EL element drive circuit) is formed on a base substrate made of an insulating material such as resin or alumina.
- the first anode electrode 2 is made of, for example, Ag (silver), APC (silver, palladium, copper alloy), ARA (silver, rubidium, gold alloy), MoCr (molybdenum and chromium alloy), or NiCr (nickel and nickel). Chrome alloy) or the like.
- Ag silver
- APC silver, palladium, copper alloy
- ARA silver, rubidium, gold alloy
- MoCr molybdenum and chromium alloy
- NiCr nickel and nickel. Chrome alloy
- the second anode electrode 3 is interposed between the first anode electrode 2 and the hole injection layer 4 and has a function of improving the bonding property between the respective layers.
- the hole injection layer 4 is preferably formed of a metal compound such as a metal oxide, a metal nitride, or a metal oxynitride.
- a metal compound such as a metal oxide, a metal nitride, or a metal oxynitride.
- the metal oxide examples include Cr (chromium), Mo (molybdenum), W (tungsten), V (vanadium), Nb (niobium), Ta (tantalum), Ti (titanium), Zr (zirconium), and Hf ( Hafnium), Sc (scandium), Y (yttrium), Th (thorium), Mn (manganese), Fe (iron), Ru (ruthenium), Os (osmium), Co (cobalt), Ni (nickel), Cu ( Copper), Zn (zinc), Cd (cadmium), Al (aluminum), Ga (gallium), In (indium), Si (silicon), Ge (germanium), Sn (tin), Pb (lead), Sb ( Antimony), Bi (bismuth), and oxides such as so-called rare earth elements from La (lanthanum) to Lu (lutetium).
- Al 2 O 3 (aluminum oxide), CuO (copper oxide), and SiO (silicon oxide) are particularly
- the bank 5 is preferably formed of, for example, an organic material such as resin or an inorganic material such as glass.
- organic materials include acrylic resins, polyimide resins, novolac type phenol resins, and examples of inorganic materials include SiO 2 (silicon oxide), Si 3 N 4 (silicon nitride), and the like. It is done.
- the bank 5 preferably has resistance to organic solvents, preferably transmits visible light to a certain degree, and preferably has insulating properties.
- an etching process or a baking process may be performed. It is suitable to form with the material with high tolerance with respect to those processes.
- the bank 5 may be a pixel bank or a line bank.
- the bank 5 is formed so as to surround the entire circumference of the organic light emitting layer 7 for each pixel.
- the bank 5 is formed so as to divide a plurality of pixels into columns or rows, and the bank 5 exists only on both sides in the row direction or both sides in the column direction of the organic light emitting layer 7. Are in the same row or row.
- the hole transport layer 6 has a function of transporting holes injected from the anode electrodes 2 and 3 to the organic light emitting layer 7.
- PEDOT poly (3,4-ethylenedioxythiophene)
- -PSS polystyrene sulfonic acid
- a derivative thereof such as a copolymer
- the organic light emitting layer 7 has a function of emitting light using an electroluminescence phenomenon, and is preferably made of, for example, a functional material included in the ink according to one embodiment of the present invention.
- the electron transport layer 8 has a function of transporting electrons injected from the cathode electrode 9 to the organic light emitting layer 7 and is preferably formed of, for example, barium, phthalocyanine, lithium fluoride, or a mixture thereof. It is.
- the cathode electrode 9 is made of, for example, ITO, IZO (indium zinc oxide) or the like. In the case of a top emission type organic light emitting device, it is preferably formed of a light transmissive material.
- the sealing layer 10 has a function of preventing the organic light emitting layer 7 or the like from being exposed to moisture or air, for example, a material such as SiN (silicon nitride) or SiON (silicon oxynitride). Formed with.
- a top emission type organic light emitting device it is preferably formed of a light transmissive material.
- the organic light-emitting element 111 and the organic display panel 110 having the above-described configuration are manufactured using the method for manufacturing an organic light-emitting element according to one embodiment of the present invention, the light-emitting characteristics are favorable.
- FIG. 17 is a diagram illustrating a schematic configuration of an ink jet apparatus according to an aspect of the present invention.
- 18 and 19 are process diagrams for describing a method for manufacturing an organic light-emitting element according to one embodiment of the present invention.
- the method for manufacturing an organic light emitting device includes first to fifth steps.
- ink according to one embodiment of the present invention is prepared, and this ink is filled into the common ink chamber 21 of the ink jet apparatus 20 according to one embodiment of the present invention as shown in FIG.
- the ink includes a functional material 22.
- the ink in the common ink chamber 21 is transported to the pressure generating chamber 24 through the ink sharing path 23.
- a part of the wall constituting the pressure generating chamber 24 is constituted by a diaphragm 25.
- the pressure generating chamber 24 is Shrink / expand.
- the ink is ejected as ink droplets 28 from the ink ejection nozzle 27 by the pressure generated by the contraction / expansion of the pressure generating chamber 24.
- a substrate 11 for preparing the organic light emitting layer 7 on which the underlayer including the first electrodes 2 and 3 is formed is prepared.
- a TFT substrate 1 whose upper surface is protected with a protective resist as shown in FIG.
- the protective resist covering the TFT substrate 1 is peeled off, an organic resin is spin-coated on the TFT substrate 1, and patterning is performed by PR / PE (photoresist / photoetching).
- PR / PE photoresist / photoetching
- a planarizing film 1a (for example, 4 ⁇ m thick) is formed.
- the first anode electrode 2 is formed on the planarizing film 1a.
- the first anode electrode 2 is formed, for example, by forming a thin film by APC by sputtering and patterning the thin film in a matrix form by PR / PE (for example, a thickness of 150 nm).
- the first anode electrode 2 may be formed by vacuum deposition or the like.
- the second anode electrode 3 is formed in a matrix.
- the second anode electrode 3 is formed, for example, by forming an ITO thin film by a plasma vapor deposition method and patterning the ITO thin film by PR / PE (for example, a thickness of 110 nm).
- a hole injection layer 4 is formed on the second anode electrode 3.
- the hole injection layer 4 is formed by sputtering a material that performs a hole injection function and patterning the material by PR / PE (for example, a thickness of 40 nm).
- the hole injection layer 4 is formed not only on the anode electrode 3 but also over the entire upper surface of the TFT substrate 1.
- a bank 5 is formed on the hole injection layer 4.
- a region where the bank 5 is formed on the hole injection layer 4 is a region corresponding to a boundary between adjacent light emitting layer forming regions.
- the bank 5 is formed by forming a bank material layer so as to cover the whole of the hole injection layer 4 and removing a part of the formed bank material layer by PR / PE (for example, a thickness of 1 ⁇ m).
- the bank 5 may be a striped line bank that extends only in the vertical direction, or may be a pixel bank that extends in the vertical and horizontal directions and has a cross-sectional shape in the form of a cross.
- the hole transport layer 6 is formed by filling the recesses between the banks 5 with ink containing the material of the hole transport layer and drying it (for example, a thickness of 20 nm). .
- the ink jet device 20 is disposed above the substrate 11, the ink is ejected as ink droplets from the ink jet device 20, and the hole facing the opening 12 between the banks 5. Ink droplets are landed on the injection layer 4.
- the filled ink droplets are dried under reduced pressure and baked to form the organic light emitting layer 7 (for example, a thickness of 60 nm to 90 nm).
- an electron transport layer 8 is formed by ETL deposition so as to cover the bank 5 and the organic light emitting layer 7 (thickness 20 nm).
- a second electrode having a polarity different from that of the first electrodes 2 and 3 is formed by plasma-depositing a light transmissive material on the organic light emitting layer 7, for example. 9 is formed (thickness 100 nm).
- a sealing layer 10 is formed by CVD from above the cathode electrode 9 (thickness 1 ⁇ m).
- FIG. 20 is a perspective view illustrating an organic display device or the like according to one embodiment of the present invention.
- the display device 100 according to one embodiment of the present invention includes an organic pixel in which pixels that emit R, G, or B light are regularly arranged in a matrix in the row direction and the column direction.
- each pixel is formed of the organic EL element according to one embodiment of the present invention.
- FIG. 21 is a diagram illustrating an overall configuration of an organic display device according to one embodiment of the present invention.
- the organic display device 100 includes an organic display panel 110 according to an aspect of the present invention, and a drive control unit 120 connected thereto.
- the drive control unit 120 is composed of four drive circuits 121 to 124 and a control circuit 125.
- the arrangement and connection relationship of the drive control unit 120 with respect to the organic display panel 110 are not limited thereto.
- the organic display device 100 having the above configuration is excellent in image quality because it uses an organic light emitting element having good light emission characteristics.
- FIG. 22A and 22B are diagrams illustrating an organic light-emitting device according to one embodiment of the present invention, in which FIG. 22A is a longitudinal sectional view, and FIG. 22B is a transverse sectional view.
- the organic light emitting device 200 includes a plurality of organic light emitting elements 210 according to one embodiment of the present invention, a base 220 on which the organic light emitting elements 210 are mounted, and organic light emission on the base 220. And a pair of reflecting members 230 attached so as to sandwich the element 210 therebetween.
- Each organic light emitting element 210 is electrically connected to a conductive pattern (not shown) formed on the base 220, and emits light by driving power supplied by the conductive pattern.
- the light distribution of a part of the light emitted from each organic light emitting element 210 is controlled by the reflecting member 230.
- the organic light emitting device 200 having the above configuration is excellent in image quality because it uses an organic light emitting element having good light emission characteristics.
- the ink for an organic light emitting device is not limited to the ink for forming the organic light emitting layer, and other than the organic light emitting layer such as a hole transport layer, an electron transport layer, a hole injection layer, and an electron injection layer.
- Ink for forming the functional layer may be used.
- the organic light emitting device is not limited to the top emission type, and may be a bottom emission type.
- the organic light-emitting layer according to one embodiment of the present invention is not described with respect to the light emission color of the organic light-emitting layer.
- the present invention can be applied not only to a single color display but also to a full color display.
- the organic light emitting elements correspond to RGB sub-pixels, and adjacent RGB sub-pixels are combined to form one pixel, and the pixels are arranged in a matrix to form an image display area. Is formed.
- the ink according to one embodiment of the present invention is not limited to an organic light emitting element, and may be an organic transistor element.
- the ink for an organic light emitting device can be widely used in a manufacturing process of an organic light emitting device by a wet process. Further, the organic light-emitting element according to one embodiment of the present invention can be widely used, for example, in the general fields of passive matrix or active matrix organic display devices and organic light-emitting devices.
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Abstract
Description
本発明の一態様に係る有機発光素子の製造方法は、機能層を構成し、重量平均分子量が0よりも大きく100000以下である機能性材料と、前記機能性材料を溶解する溶媒とを含むインクを準備し、前記インクを、インク吐出ノズルを備えたインクジェット装置に充填する第1工程と、第1電極を含む下地層が形成された基板を準備する第2工程と、前記インクジェット装置を前記基板の上方に配置し、前記インクジェット装置から前記インクをインク液滴として吐出させ、前記基板の前記下地層上に前記インク液滴を着弾させる第3工程と、前記インク液滴を乾燥させ、前記機能層を形成する第4工程と、前記機能層の上方に、第2電極を形成する第5工程と、
を有し、前記第1工程における前記インクの密度ρ(g/m3)、表面張力γ(mN・m)および粘度η(mPa・s)、並びに、前記インク吐出ノズルのノズル径r(mm)が、上記[数1]のZ(オーネゾルゲ数Ohの逆数)の数値範囲を満たし、前記第3工程における前記インク液滴の吐出速度V(m/s)が、上記[数2]の数値範囲を満たし、前記Zの値と前記吐出速度V(m/s)とが、上記[数3]の関係式を満たすように設定する、ことを特徴とする。
発明者は、好適な飛翔特性となる条件を簡単かつ正確に推測できる技術を、以下に説明する実験・考察を経て完成させた。
まず、好適な飛翔特性となる条件を簡単かつ正確に推測するために、どのような変数で飛翔特性をコントロールすれば良いのかを検討するにあたって、インクの挙動に影響を与える3種類の物理的な力(粘性抵抗、慣性力、表面張力)に着眼して考察を行なった。
慣性力は、下記[式2]に示すように、インク密度ρ、インク液滴径r’、吐出速度Vにより定まる。
表面張力は、下記[式3]に示すように、インク表面張力γ、インク液滴径r’により定まる。
総括すると、インク液滴の飛翔特性に影響を与える要因としては、インク密度ρ、インク表面張力γ、インク粘度η、インク液滴径r’および吐出速度Vの5つが挙げられる。これら5つの要因のうち、インク密度ρ、インク表面張力γ、インク粘度ηおよびインク液滴径r’の4つの要因は、インク物性に関する要因であり、吐出速度Vだけがインク物性以外の要因である。これら要因の全てを変数とすると、変数が5つにもなり、しかもそれらは相互関係が不明であるため、飛翔特性のコントロールが非常に困難である。
ウェーバー数Nweとは、二相流を扱う際に重要な無次元数であり、液滴が気流中を流れる場合の変形挙動や、液滴の界面の安定性問題の整理に利用される値である。本願ではインク液滴の***性に主として関与すると考えられる。ウェーバー数Nweは、下記[式5]に示すように、慣性力と表面張力との比で表される。
オーネゾルゲ数(Ohnesorge number)Ohとは、粘性力と、慣性力および表面張力との関係を示す無次元数である。オーネゾルゲ数Ohは、下記[式6]に示すように、レイノルズ数Nreとウェーバー数Nweとの比で表される。
ここで、上記[式6]に[式4]および[式5]を代入すれば、下記[式7]に示すように、粘性抵抗、慣性力、表面張力の3つの力のバランスを、インク物性に関するインク密度ρ、インク表面張力γ、インク粘度ηおよびインク液滴径r’の4つの要因だけで表すことが可能になり、インク物性以外の要因である吐出速度Vを打ち消すことができる。さらに、インク物性に関する4つの要因は、オーネゾルゲ数Ohの逆数であるZ値でひとまとめに表すことができる。
=レイノルズ数Nre/(ウェーバー数Nwe)1/2
=(慣性力/粘性力)/(慣性力/表面張力)1/2
=(v・r・ρ/η)/(v2・r・ρ/γ)1/2
=(r・ρ・γ)1/2/η …[式7]
このように、飛翔特性に影響を及ぼす要因を、インク物性に関する要因と、インク物性以外の要因とに分け、さらに、インク物性に関する要因をひとまとめにしたZ値を1つの変数として扱えば、飛翔特性のコントロールが非常に容易である。
飛翔特性が好適だと言えるためには、インク液滴の直進性が良好でなければならない。直進性が良好であるとは、インクジェット装置から吐出されたインク液滴が真っ直ぐに目的の位置まで到達することを意味する。直進性は、例えばインク液滴の着弾精度を測定して評価することができる。
吐出速度Vと飛翔特性との相関性の検討は、吐出速度Vとインク液滴の直進性(着弾精度)との関係を調べることにより行なった。測定用のインクは、機能性材料としてF8-F6を用い、溶媒としてシクロヘキシルベンゼン、メトキシトルエン、1-ノナノール、ジメチルフタレート、アセトフェノン、キシレンのいずれかを用いた。そして、各種インクをインク吐出ノズルから種々の吐出速度Vで吐出させ、それらの着弾精度を測定し、標準偏差6σで評価した。なお、吐出速度Vとして、インクジェット評価装置Litrex120L(株式会社アルバック製)を用いて、インクジェットヘッド先端から0.5mmの液滴の速度を測定した。
ところで、上記実験において、吐出速度Vを大きくしていくと、インクが***してサテライトが発生し、飛翔特性を損なうことがわかった。インク液滴の飛翔特性が好適だと言えるためには、***性も良好でなければならない。インク液滴の***性が良好であるとは、インク液滴が***しないことを意味する。
当初の考察からすれば、Z値および吐出速度Vのそれぞれの変数について実験確認をおこない、相関性を示す関係式が得られれば、飛翔特性をコントロールするのに十分だと思われた。しかしながら、インク液滴の***性の点から、吐出速度Vに上限値が存在することが判明したことより、Z値とインク液滴の***性との間にも何らかの相関性が存在すると推測し、さらに検討を進めた。
図13のグラフにおいて回帰線よりも下側の領域がサテライトの発生しない領域である。そして、Z値が13を超えた場合にサテライト発生速度が3.0(m/s)未満になることが分かる。したがって、Z値の上限を13と定めた。
以上のように、インク液滴の***性は、吐出速度Vのみに依存する訳ではなく、吐出速度VとZ値の両方の変数に依存しており、それ故、インク液滴の***性を良好にするためには、Z値と吐出速度Vとが所定の関係を満たすことが重要であることが判明した。
本発明の一態様に係るインクは、機能層を構成する機能性材料と、当該機能性材料を溶解する溶媒とを含み、インクジェット装置を用いたインクジェット法(液滴吐出法)に適したインク物性を有する。そのようなインク物性としては、図3および図12から分かるように、インク密度ρは827(g/m3)よりも大きく1190(g/m3)以下、インク表面張力γは27.3(mN・m)よりも大きく41.9(mN・m)以下、インク粘度ηは2.4(mPa・s)よりも大きく35.0(mPa・s)以下であることが好適である。その場合、インクジェット装置のインク吐出ノズルのノズル径rは、0.02(mm)以上0.03(mm)以下であることが好適である。
図16は、本発明の一態様に係る有機表示パネルの各層の積層状態を示す模式図である。図16に示すように、本発明の一態様に係る有機表示パネル110は、本発明の一態様に係る有機発光素子111上にシール材112を介してカラーフィルター基板113を貼り合わせた構成を有する。
図17~図19に基づいて、本発明の一態様に係るインクジェット装置および有機発光素子の製造方法を説明する。図17は、本発明の一態様に係るインクジェット装置の概略構成を示す図である。図18および図19は、本発明の一態様に係る有機発光素子の製造方法を説明するための工程図である。
図20は、本発明の一態様に係る有機表示装置等を示す斜視図である。図20に示すように、本発明の一態様に係る表示装置100は、R、G、又はBの光を出射する各ピクセルが行方向及び列方向にマトリックス状に規則的に配置されてなる有機ELディスプレイであって、各ピクセルが本発明の一態様に係る有機EL素子で構成されている。
図22は、本発明の一態様に係る有機発光装置を示す図であって、(a)は縦断面図、(b)は横断面図である。図22に示すように、有機発光装置200は、本発明の一態様に係る複数の有機発光素子210と、それら有機発光素子210が上面に実装されたベース220と、当該ベース220にそれら有機発光素子210を挟むようにして取り付けられた一対の反射部材230と、から構成されている。各有機発光素子210は、ベース220上に形成された導電パターン(不図示)に電気的に接続されており、前記導電パターンにより供給された駆動電力によって発光する。各有機発光素子210から出射された光の一部は、反射部材230によって配光が制御される。
以上、本発明の一態様に係る有機発光素子の製造方法、有機表示パネル、有機発光装置、機能層の形成方法、インク、基板、有機発光素子、有機表示装置および、インクジェット装置を具体的に説明してきたが、上記実施の形態は、本発明の構成および作用・効果を分かり易く説明するために用いた例であって、本発明の内容は、上記の実施の形態に限定されない。
5 隔壁
6 機能層
9 第2電極
11 基板
12 開口
20 インクジェット装置
22 機能性材料
27 インク吐出ノズル
100 有機発光装置
110 有機表示パネル
111 有機発光素子
200 有機表示装置
Claims (26)
- 機能層を構成し、重量平均分子量が0よりも大きく100000以下である機能性材料と、前記機能性材料を溶解する溶媒とを含むインクを準備し、前記インクを、インク吐出ノズルを備えたインクジェット装置に充填する第1工程と、
第1電極を含む下地層が形成された基板を準備する第2工程と、
前記インクジェット装置を前記基板の上方に配置し、前記インクジェット装置から前記インクをインク液滴として吐出させ、前記基板の前記下地層上に前記インク液滴を着弾させる第3工程と、
前記インク液滴を乾燥させ、前記機能層を形成する第4工程と、
前記機能層の上方に、第2電極を形成する第5工程と、
を有し、
前記第1工程における前記インクの密度ρ(g/m3)、表面張力γ(mN・m)および粘度η(mPa・s)、並びに、前記インク吐出ノズルのノズル径r(mm)が、下記[数1]のZ(オーネゾルゲ数Ohの逆数)の数値範囲を満たし、
前記第3工程における前記インク液滴の吐出速度V(m/s)が、下記[数2]の数値範囲を満たし、
前記Zの値と前記吐出速度V(m/s)とが、下記[数3]の関係式を満たすように設定する、
ことを特徴とする有機発光素子の製造方法。
- 前記Zの値は、2以上10以下であり、
前記吐出速度Vは、3(m/s)以上5(m/s)以下である、請求項1記載の有機発光素子の製造方法。 - 前記インクの密度ρは、827(g/m3)よりも大きく1190(g/m3)以下であり、
前記インクの表面張力γは、27.3(mN・m)よりも大きく41.9(mN・m)以下であり、
前記インクの粘度ηは2.4(mPa・s)よりも大きく35.0(mPa・s)以下であり、
前記インクジェット装置のノズル径rは、0.02(mm)以上0.03(mm)以下である、
請求項1記載の有機発光素子の製造方法。 - 前記第2工程は、画素部に対応する開口を備え、隣り合う画素部を区画する複数の隔壁を前記下地層の上方に有する基板を準備し、
前記第3工程は、前記基板の前記隔壁間の開口に面する下地層上に、前記インク液滴を着弾させる、
請求項1記載の有機発光素子の製造方法。 - 請求項1記載の有機発光素子の製造方法により製造された有機発光素子を用いた有機表示パネル。
- 請求項1記載の有機発光素子の製造方法により製造された有機発光素子を用いた有機発光装置。
- 請求項1記載の有機発光素子の製造方法により製造された有機発光素子を用いた有機表示装置。
- 機能層を構成し、重量平均分子量が0よりも大きく100000以下である機能性材料と、前記機能性材料を溶解する溶媒とを含むインクを準備し、前記インクを、インク吐出ノズルを備えたインクジェット装置に充填する第1工程と、
前記機能層を形成するための基板を準備する第2工程と、
前記インクジェット装置を前記基板の上方に配置し、前記インクジェット装置から前記インクをインク液滴として吐出させ、前記基板上に前記インク液滴を着弾させる第3工程と、
前記インク液滴を乾燥させ、前記機能層を形成する第4工程と、
を有し、
前記第1工程における前記インクの密度ρ(g/m3)、表面張力γ(mN・m)および粘度η(mPa・s)、並びに、前記インク吐出ノズルのノズル径r(mm)が、下記[数1]のZ(オーネゾルゲ数Ohの逆数)の数値範囲を満たし、
前記第3工程における前記インク液滴の吐出速度V(m/s)が、下記[数2]の数値範囲を満たし、
前記Zの値と前記吐出速度V(m/s)とが、下記[数3]の関係式を満たすように設定する、
ことを特徴とする機能層の形成方法。
- 前記Zの値は、2以上10以下であり、
前記吐出速度Vは、3(m/s)以上5(m/s)以下である、
請求項8記載の機能層の形成方法。 - 前記インクの密度ρは、827(g/m3)よりも大きく1190(g/m3)以下であり、
前記インクの表面張力γは、27.3(mN・m)よりも大きく41.9(mN・m)以下であり、
前記インクの粘度ηは2.4(mPa・s)よりも大きく35.0(mPa・s)以下であり、
前記インクジェット装置のノズル径rは、0.02(mm)以上0.03(mm)以下である、請求項8記載の機能層の形成方法。 - インク吐出ノズルを備えたインクジェット装置を用いて吐出され、基板上に着弾して乾燥させられて機能層を構成するためのインクであって、
前記機能層を構成し、重量平均分子量が0よりも大きく100000以下である機能性材料と、前記機能性材料を溶解する溶媒とを含み、
その密度ρ(g/m3)、その表面張力γ(mN・m)およびその粘度η(mPa・s)、並びに、前記インク吐出ノズルのノズル径r(mm)が、下記[数1]のZ(オーネゾルゲ数Ohの逆数)の数値範囲を満たし、
前記インクジェット装置から下記[数2]の数値範囲を満たす吐出速度V(m/s)で吐出され、
前記吐出速度V(m/s)に対して、前記Zの値が下記[数3]の関係式を満たす、
ことを特徴とするインク。
- 有機発光素子の機能層を構成する機能性材料と、溶媒とを含み、
第1電極を含む下地層が形成された有機発光素子用基板における、前記下地層上に着弾して乾燥され、前記第1電極と、前記下地層に対向する第2電極との間において有機発光素子の機能層を構成するためのインクである、請求項11記載のインク。 - 前記密度ρ(g/m3)、前記表面張力γ(mN・m)、および、前記粘度η(mPa・s)は前記吐出速度Vが3(m/s)以上5(m/s)以下において、前記Zの値が2以上10以下を満たすように設定されている、請求項11記載のインク。
- 前記インクジェット装置のノズル径rが、0.02(mm)以上0.03(mm)以下において、
前記密度ρは、827(g/m3)よりも大きく1190(g/m3)以下であり、
前記表面張力γは、27.3(mN・m)よりも大きく41.9(mN・m)以下であり、
前記粘度ηは2.4(mPa・s)よりも大きく35.0(mPa・s)以下である、
請求項11記載のインク。 - 前記請求項11記載のインクを用いて製造された、機能層を有する基板。
- 前記請求項12記載のインクを用いて製造された、機能層を有する有機発光素子。
- 請求項12記載のインクを用いて製造された、機能層を有する有機発光素子を備える有機表示パネル。
- 請求項12記載のインクを用いて製造された、機能層を有する有機発光素子を備える有機発光装置。
- 請求項12記載のインクを用いて製造された、機能層を有する有機発光素子を備える有機表示装置。
- 機能層を構成し、重量平均分子量が0よりも大きく100000以下である機能性材料と、前記機能性材料を溶解する溶媒とを含むインクを収容し、
前記インクをインク吐出ノズルから吐出し、基板上に着弾させて機能層を形成するためのインクジェット装置であって、
前記インク吐出ノズルのノズル径r(mm)は、
前記インクの密度ρ(g/m3)、表面張力γ(mN・m)、および、粘度η(mPa・s)に対して、下記[数1]のZ(オーネゾルゲ数Ohの逆数)の数値範囲を満たし、
前記インクを吐出する吐出速度V(m/s)は、
下記[数2]の数値範囲を満たし、さらに、前記Zの値に対して、下記[数3]の関係式を満たす、
ことを特徴とする、インクジェット装置。
- 前記インクの機能性材料は、有機発光素子の機能層を構成する機能性材料であり、
前記インクを吐出し、前記インクを第1電極を含む下地層が形成された有機発光素子用基板における前記下地層上に着弾させ、前記第1電極と、前記下地層に対向する第2電極との間において前記有機発光素子の前記機能層を形成するためのインクジェット装置である、請求項20記載のインクジェット装置。 - 前記請求項20記載のインクジェット装置を用いて製造された、機能層を有する基板。
- 前記請求項21記載のインクジェット装置を用いて製造された、機能層を有する有機発光素子。
- 請求項21記載のインクジェット装置を用いて製造された、機能層を有する有機発光素子を備える有機表示パネル。
- 請求項21記載のインクジェット装置を用いて製造された、機能層を有する有機発光素子を備える有機発光装置。
- 請求項21記載のインクジェット装置を用いて形成された、機能層を有する有機発光素子を備える有機表示装置。
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JPWO2012098578A1 (ja) | 2014-06-09 |
US8980678B2 (en) | 2015-03-17 |
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