Method for controlling micro-pollution residues of OLED organic evaporation cavity components

Abstract

The present application relates to the field of integrated circuit manufacturing technology, and in particular to a method for controlling micro-pollution residues of OLED organic evaporation cavity components. The present application simulates the vacuum operating environment in the OLED organic evaporation process, compares and analyzes the physical and chemical properties of the organic material and the cavity components, and the evaporation conditions and other factors of the organic evaporation environment temperature, and designs a method suitable for wide popularization and greatly reducing the micro-pollution residues of the organic evaporation cavity components.

Description

Technical Field

[0001] This application relates to the field of integrated circuit manufacturing technology, and more specifically, it relates to a method for controlling micro-contamination residues in OLED organic vapor deposition cavity components. Background Technology

[0002] In the field of OLED displays, organic vapor deposition is one of the most important production processes. The selection of materials, parameter settings, equipment chamber structure, and control of micro-contamination residues in organic vapor deposition directly affect the production yield and luminous efficiency of OLED display devices. During the OLED manufacturing process, organic vapor deposition materials vaporize in the process chamber and adhere to the surface of the glass substrate to form the corresponding light-emitting display layer device structure. These organic vapor deposition materials accumulate in large quantities inside the chamber after each use, requiring periodic cleaning and reuse. This leads to difficulties in identifying micro-contamination residues and numerous influencing factors.

[0003] For a long time, controlling the residue of organic vapor deposition materials has been a difficult and important issue in the OLED production process. The traditional control method is to disassemble the equipment cavity components and then soak and wipe them in the atmosphere with organic solvents. However, molecular or ionic solutions can easily penetrate into the product. During the process, this method has problems such as organic material residue, solvent residue and environmental particulate matter, which have a significant impact on the production quality of OLED display devices. Summary of the Invention

[0004] In order to solve the technical problems of difficult identification of micro-contamination residues, organic material residues, and solvent residues caused by traditional control methods, the purpose of this invention is to provide a method for controlling micro-contamination residues in OLED organic vapor deposition cavity components.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] A method for controlling micro-contamination residues in OLED organic vapor deposition cavity components includes the following steps:

[0007] S1: Pre-treat the cavity components in an organic solvent;

[0008] S2: Place the pre-treated cavity components into pure water and perform ultrasonic immersion cleaning and pre-drying treatment in sequence.

[0009] S3: Take an appropriate amount of the pure water after ultrasonic cleaning in step S2 and test its COD. The test result must be less than 1.0 ppm. If it fails, repeat step S2.

[0010] S4: Perform surface treatment on the cavity components that have passed the COD test;

[0011] S5: Immerse the surface-treated cavity components in pure water for multi-stage ultrasonic immersion cleaning, with an ultrasonic energy density of 12–18 W / inch. 2 The pure water temperature is controlled at 25-28℃, the time is controlled at 45-60 minutes, and the working environment is a Class 1000 or Class 100 cleanroom.

[0012] S6: After the cavity components have been cleaned by multi-stage ultrasonic immersion, they are placed in a vacuum oven for drying. The vacuum level is controlled at 0.1 to 0.01 Pa, and the working environment is a Class 100 cleanroom.

[0013] S7: Perform residual testing on the cavity components after vacuum baking, including IC, ICP-MS, and surface particle size analysis. For IC-related tests, the ion solubility of Cl, NO3, and F ions must be less than 1.0 mg / L. For ICP-MS-related tests, the results for Al, Na, Mg, K, and C must be less than 1.0 ppm. Surface particle size analysis must be ≥0.3 μm and ≤1 ea / cm. 2 ;

[0014] S8: If the residue test results exceed the standard, repeat steps S5 to S7;

[0015] S9: Select packaging materials that meet the requirements for micro-contamination control and vacuum-pack the qualified components.

[0016] Optionally, the preprocessing in step S1 includes the following steps:

[0017] S11: Disassemble and remove the cavity components attached to the organic film layer inside the OLED organic vapor deposition cavity, and place them in a dedicated turnover vehicle.

[0018] S12: Transport the cavity components to the cleaning area for high-pressure water jet cleaning, with the high-pressure water jet pressure controlled at 14500psi~17500psi;

[0019] S13: After the high-pressure water jet operation, the cavity components are sequentially placed into three ultrasonic immersion tanks. The tank solution temperature is controlled at 55-65℃, and the solution consists of 99.85% NMP and 99.9% DMAC. The immersion times are 2 hours, 1 hour, and 1 hour, respectively, supplemented with an energy density of 12-18 W / inch. 2 The ultrasonic vibration.

[0020] Optionally, in step S13, the bath solution is composed of 99.85% NMP and 99.9% DMAC in a volume ratio of (6.3 to 7.7):2.

[0021] Optionally, in step S2, the ultrasonic energy density is 12–18 W / inch.2 The temperature of the bath solution is controlled at 95-98℃, and the time is controlled at 45-60 minutes.

[0022] Optionally, in step S2, the baking temperature of the pre-drying treatment is controlled at 180-200°C, and the time is controlled at 45-60 min.

[0023] Optionally, in step S4, the surface treatment includes protection, sandblasting, and inspection and correction procedures.

[0024] Optionally, in step S6, the temperature curve of the vacuum oven is set to gradually increase from room temperature to 450°C, hold at that temperature for 4 hours, and then allow it to cool naturally.

[0025] In summary, this application has the following beneficial effects: By simulating the vacuum working environment in the OLED organic vapor deposition process, comparing and analyzing the physicochemical properties of organic materials and cavity components, as well as various factors such as the temperature and evaporation conditions of the organic vapor deposition environment, the vacuum baking temperature used in the process is higher than the process temperature in the OLED display device manufacturing process. The reason is that the high temperature zone in the vapor deposition cavity is concentrated at the evaporation source position, while the temperature in other parts of the cavity is relatively low and more film and contaminant deposits are formed. Under this temperature condition, the removal effect of organic residues and micro-contaminations on the surface of the cavity components can be more ideal. Thus, a control method suitable for widespread application and minimizing micro-contamination residues in organic vapor deposition cavity components is designed. Attached Figure Description

[0026] Figure 1 This is the control flowchart of the present invention;

[0027] Figure 2 This is a temperature curve of the vacuum oven in this invention. Detailed Implementation

[0028] The present application will be further described in detail below with reference to the accompanying drawings and embodiments.

[0029] A method for controlling micro-contamination residues in OLED organic vapor deposition cavity components, characterized by comprising the following steps:

[0030] S1: Pre-treatment of the cavity components by immersing them in an organic solvent, specifically including the following steps:

[0031] S11: After one cycle of use, the cavity components with organic film attached to them in the OLED organic vapor deposition cavity are disassembled and removed, and placed in a dedicated turnover vehicle to avoid stacking and collision, and to prevent deformation or changes in surface roughness of the cavity components.

[0032] S12: Transport the cavity components to the cleaning area for high-pressure water jet cleaning. The high-pressure water jet pressure is controlled at 14500psi~17500psi. Because organic dust and wastewater containing organic materials will be generated during the operation, the operation environment must be selected in an area with the ability to treat dust exhaust gas and organic wastewater. During cleaning, the area where organic materials are attached should be swept evenly to promote the extensive peeling of the surface film layer of the cavity components.

[0033] S13: After the high-pressure water jetting operation, the cavity components are sequentially placed into three ultrasonic soaking tanks. The temperature of the tank solution is controlled at 55-65℃. The tank solution consists of 99.85% NMP (N-methylpyrrolidone) and 99.9% DMAC (dimethylacetamide) in a volume ratio of (6.3-7.7):2, preferably 7:2. The cavity components are soaked in the three ultrasonic soaking tanks for 2 hours, 1 hour, and 1 hour, respectively. Each ultrasonic soaking tank is supplemented with an energy density of 12-18 W / inch. 2 Ultrasonic oscillation;

[0034] S2: Place the pre-treated cavity components into a pure water immersion tank for ultrasonic pure water immersion. The ultrasonic energy density is 12-18 W / inch. 2 The pure water temperature is controlled at 95-98℃, and the time is controlled at 45-60 minutes. During this period, attention should be paid to the placement angle of the cavity components to avoid stacking. Then, the cleaned cavity components are placed in a drying oven for pre-drying treatment. The baking temperature is controlled at 180-200℃, and the time is controlled at 45-60 minutes.

[0035] S3: Take an appropriate amount of the pure water after ultrasonic cleaning in step S2 and test it for COD (chemical oxygen demand). The test result should be less than 1.0 ppm. If it fails, repeat step S2.

[0036] S4: After the COD test is passed, the cavity components will undergo surface treatment. Surface treatment includes protection, sandblasting, inspection and correction and other operations. The specific parameters are related to the structure and surface properties of the cavity components, and will not be described in detail here.

[0037] S5: Place the surface-treated cavity components sequentially into multiple pure water immersion tanks for multi-stage ultrasonic immersion cleaning. The ultrasonic energy density in any pure water immersion tank is 12-18 W / inch. 2 The pure water temperature is controlled at 25-28℃, the time is controlled at 45-60 minutes, and the working environment is a Class 1000 or Class 100 cleanroom. During the process, pay attention to the placement angle of the cavity components to avoid the problem of stacking, which will reduce the particle cleaning effect.

[0038] S6: After multi-stage ultrasonic immersion cleaning, the cavity components are placed in a vacuum oven for drying. The operating environment is a Class 100 cleanroom. The temperature profile is set to gradually increase from room temperature to 450℃, maintain the temperature for 4 hours, and then allow natural cooling. Figure 2 As shown), the vacuum degree is controlled at 0.1 to 0.01 Pa. Note that the evaporation temperature of organic materials is 300 to 400°C. The cavity components are made of high-temperature resistant metals such as molybdenum, stainless steel, and titanium alloy. The actual temperature conditions should not exceed 500°C to prevent changes in the stress structure of the cavity components and changes in the surface microstructure under high temperature conditions.

[0039] S7: Perform residual detection on the cavity components after vacuum baking, including IC (ion chromatography), ICP-MS (inductively coupled plasma mass spectrometry), and surface particle size analysis. Specifically, the ion solubility of Cl, NO3, and F ions related to IC must be less than 1.0 mg / L; the detection results of Al, Na, Mg, K, and C related to ICP-MS must be less than 1.0 ppm; and the surface particle size must be ≥0.3 μm and ≤1 ea / cm. 2 ;

[0040] S8: If the residue test results exceed the standard, repeat steps S5 to S7;

[0041] S9: Select packaging materials that meet the requirements for micro-contamination control and vacuum-pack the qualified components.

[0042] In step S6, the vacuum condition ensures that the organic material vaporizes rather than carbonizes after reaching the evaporation temperature. The 450°C temperature condition can not only remove material residues but also ensure the stability of the cavity component material and structure (the melting point of materials such as molybdenum, stainless steel, and titanium alloys is above 800°C). Baking for 4 hours ensures that the residues inside the material are fully removed. In actual production, the parameters can be fine-tuned.

[0043] The technical features of the above embodiments can be combined arbitrarily. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as the combination of these technical features does not contradict each other, it should be considered to be within the scope of this specification.

[0044] The above specific embodiments are merely explanations of this application and are not intended to limit this application. After reading this specification, those skilled in the art can make modifications to these embodiments without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A method for controlling micro-contamination residues in OLED organic vapor deposition cavity components, characterized in that, Includes the following steps: S1: Pre-treat the cavity components in an organic solvent; S2: Place the pre-treated cavity components into pure water and perform ultrasonic immersion cleaning and pre-drying treatment in sequence. S3: Take an appropriate amount of the pure water after ultrasonic cleaning in step S2 and test its COD. The test result must be less than 1.0 ppm. If it fails, repeat step S2. S4: Perform surface treatment on the cavity components that have passed the COD test; S5: Put the surface treated cavity parts into pure water, and perform multi-stage ultrasonic immersion cleaning, with ultrasonic energy density of 12-18 w / inch 2 , pure water temperature controlled at 25-28℃, time controlled at 45-60 min, and operation environment controlled at 1000-level or 100-level dust-free room; S6: After the cavity components have been cleaned by multi-stage ultrasonic immersion, they are placed in a vacuum oven for drying. The vacuum level is controlled at 0.01 to 0.1 Pa, and the working environment is a Class 100 cleanroom. S7: Perform residual detection on cavity components after vacuum baking, including IC, ICP-MS, and surface particle size analysis, among which IC-related... The ion concentration detection results must all be less than 1.0 mg / L, and the detection results of Al, Na, Mg, K, and C related to ICP-MS must all be less than 1.0 ppm. The surface particle size detection results must be ≥0.3 μm and ≤1 ea / cm. 2 Among them, "the surface particle size must be ≥0.3μm and ≤1ea / cm". 2 The meaning of "" is "the detection value of particles with a particle size ≥0.3um on the surface of the component is ≤1 particle per square centimeter"; S8: If the residue test results exceed the standard, repeat steps S5 to S7; S9: Select packaging materials that meet the requirements for micro-contamination control and vacuum-pack the qualified components; The preprocessing in step S1 includes the following steps: S11: Disassemble and remove the cavity components with organic film layers attached to them in the OLED organic vapor deposition cavity and place them in a turnover cart; S12: Transport the cavity components to the cleaning area for high-pressure water jet cleaning, with the high-pressure water jet pressure controlled at 14500psi~17500psi; S13: the cavity parts after the high-pressure water jet operation are sequentially put into three ultrasonic soaking tanks, the tank liquid temperature is controlled at 55-65°C, the tank liquid is composed of 99.85% NMP and 99.9% DMAC, the soaking time is 2H, 1H and 1H respectively, and is supplemented with ultrasonic oscillation with an energy density of 12-18 w / inch 2 ; In step S13, the bath solution is composed of 99.85% NMP and 99.9% DMAC in a volume ratio of (6.3~7.7):2; In step S4, the surface treatment includes protection, sandblasting, and inspection and correction procedures.

2. The control method according to claim 1, characterized in that, In step S2, the ultrasonic energy density is 12–18 W / inch. 2 The temperature of the bath solution is controlled at 95-98℃, and the time is controlled at 45-60 minutes.

3. The control method according to claim 1, characterized in that, In step S2, the baking temperature for the pre-drying treatment is controlled at 180–200°C, and the time is controlled at 45–60 min.

4. The control method according to claim 1, characterized in that, In step S6, the temperature curve of the vacuum oven is set to gradually increase from room temperature to 450°C, hold the temperature for 4 hours, and then cool down naturally.

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