A method for preparing an ultra-smooth organic film layer

Abstract

The application discloses a preparation method of an ultra-smooth organic film layer. The film coating is carried out on the surface of inorganic film layers such as silicon oxide and aluminum oxide, and the process comprises three process procedures of organic matter flashing, organic matter flowing and organic film layer polymerization. The organic film layer prepared by the method has the following effects: on the one hand, the inorganic film layer is planarized, and the roughness is reduced from 20 nm to within 3 nm; and on the other hand, the organic layer can compensate for microscopic defects such as pinholes and micro-cracks, prolong the path of gas molecules, and can prepare a high-barrier thin film. The organic diaphragm prepared by the application is obtained by flashing through the winding method on the surface of the oxide film layer, the thin film product has the ultra-smooth characteristic, the roughness is less than 3 nm by using an atomic force microscope, and can be applied in the fields of quantum dot display, photovoltaic, photoelectric material packaging and barrier film.

Description

TECHNICAL FIELD

[0001] The application relates to a preparation method of an ultra-smooth organic film layer and belongs to the technical field of organic film layer preparation. BACKGROUND

[0002] With the proposal of the concept of "flexible+" and the rapid development of technology, the demand for packaging barrier films and preparation technology thereof, which are key raw materials for the production of high-tech products such as quantum dot display, OLED display and thin-film solar cell and have the characteristics of spectral transparency, high barrier property and high flexibility, is becoming more and more urgent. Taking OLED as an example, the barrier ability (oxygen transmission rate, water vapor transmission rate) of the packaging film selected by the OLED is a main factor affecting the performance and service life of the light-emitting diode. Therefore, with the development of OLED, quantum dot display, OPV (organic solar cell) and other high-value-added industries such as flexible electronics, the market prospect of high-index and extremely high-index packaging film products, preparation technology and related equipment will be very huge.

[0003] Preparation of high-index water vapor and oxygen barrier film (10 -3 The mainstream technical route for preparing the packaging material is an organic / inorganic laminated scheme, and a typical structure of the barrier film lamination is 50-100 mu m PET / organic layer / inorganic barrier layer / organic layer. The inorganic layer has high barrier performance, and the organic layer can flatten the inorganic film layer and fill the pinholes, microcracks and other defects of the inorganic layer on the other hand. The flattening degree of the organic film layer determines the index level of the barrier layer. SUMMARY

[0004] The application aims to provide a preparation method of an ultra-smooth organic film layer, which has the characteristics of surface ultra-smoothness and extremely low roughness, to meet the demand of flexible electronic packaging technology.

[0005] The application is achieved in the following manner:

[0006] The application provides a preparation method of an ultra-smooth organic film layer, which adopts a roll-type vacuum evaporation film plating machine. The film plating process comprises organic flash evaporation, organic flow flattening and organic film layer polymerization. The method steps are as follows:

[0007] Firstly, the base film is installed. A 12-125 mu m thick polyester film (PET) is pre-grown with a 60-180 nm oxide film to obtain a film to be plated, and the film to be plated is installed on a unwinding roller of the roll-type vacuum evaporation film plating machine.

[0008] Secondly, the vacuum chamber is evacuated. The roll-type vacuum evaporation film plating machine with the film to be plated installed in the first step is evacuated, so that the background vacuum degree is better than 3x10 -3 Pa;

[0009] Third step, ion source pretreatment: start the roll vacuum evaporation coating machine to start winding, start the anode layer ion source, pretreat the surface to be coated, and adjust the wetting tension of the surface to be coated to 44-56 dynes;

[0010] Fourth step, coating polyacrylate film layer: using methyl acrylate, liquid flow meter control 0.5-5ml / min flow, evaporator temperature 150-300℃;

[0011] Fifth step, ultraviolet lamp curing, power 200-1000W, vacuum degree control at 1-2Pa, base film winding speed 50-500mm / min, to get super smooth organic film layer.

[0012] The oxide film is a silicon oxide inorganic film layer or an aluminum oxide inorganic film layer.

[0013] Beneficial effects

[0014] (1) The application discloses a preparation method of a super smooth organic film layer. The coating is performed on the surface of an inorganic film layer such as a silicon oxide film or an aluminum oxide film, and the process comprises three process procedures of organic matter flashing, organic matter flow leveling and organic film layer polymerization.

[0015] (2) The organic film layer prepared by the method has the effects of planarizing the inorganic film layer, reducing the roughness from 20nm to below 3nm, and compensating for microscopic defects such as pinholes and microcracks, prolonging the path of gas molecules and enabling the preparation of a high-barrier thin film.

[0016] (3) The organic separator prepared by the application is obtained by flashing through winding on the surface of the oxide film layer, and the thin film product has super smooth characteristics, the roughness is less than 3nm as tested by an atomic force microscope, and can be applied to the fields of quantum dot display, photovoltaic and photoelectric material packaging barrier films.

[0017] (4) The application discloses a preparation method of a super smooth organic film layer. The organic film layer is prepared by a vacuum evaporation method, the raw material of the organic layer is an acrylate lipid, and the process procedure of vacuum flashing, flow leveling and ultraviolet curing is adopted; the coating equipment is a self-developed roll-to-roll vacuum flashing equipment, and the coating of the organic film layer is completed in a vacuum environment; the multi-layer barrier film product has super smooth characteristics, the roughness is less than 3nm as tested by an atomic force microscope, and can be applied to the fields of quantum dot display, photovoltaic and photoelectric material packaging barrier films.

[0018] (5) The super smooth organic film prepared by the method supports the technical development of flexible electronic super high barrier film packaging materials. The vacuum flashing coating method can be used in the same chamber as the inorganic oxide film layer to realize "one-time film forming" and improve the production efficiency. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 Figure 1 is an AFM surface topography diagram of the organic layer after plating. DETAILED DESCRIPTION

[0020] The application will be further described in conjunction with the accompanying drawings and examples.

[0021] A method for preparing an ultra-smooth organic film layer, using a roll-type vacuum evaporation film plating machine, the film plating process including organic flash evaporation, organic flow leveling, organic film layer polymerization, etc., the method steps being as follows:

[0022] Step 1: Base film installation: using 12-125 micron thick polyester film (PET) pre-grown with 60-180 nm oxide film, obtaining a film to be plated, and installing the obtained film to be plated on the unwinding roller of the roll-type vacuum evaporation film plating machine.

[0023] Step 2: Vacuum chamber vacuum pumping: vacuum pumping the roll-type vacuum evaporation film plating machine with the film to be plated installed in Step 1, so that the base vacuum degree is better than 3x10 -3 Pa.

[0024] Step 3: Ion source pretreatment: starting winding of the roll-type vacuum evaporation film plating machine, starting the anode layer ion source, pretreating the surface of the film to be plated, and adjusting the wetting tension of the surface of the film to be plated to 44-56 dynes.

[0025] Step 4: Plating polyacrylate film layer: using methyl acrylate, liquid flow meter control 0.5-5 ml / min flow, evaporator temperature 150-300℃.

[0026] Step 5: Ultraviolet lamp curing, power 200-1000W, vacuum degree controlled at 1-2Pa, base film winding speed 50-500mm / min, obtaining an ultra-smooth organic film layer.

[0027] The oxide film is a silicon oxide inorganic film layer or an aluminum oxide inorganic film layer.

[0028] The application uses a vacuum flash evaporation method to plate an ultra-smooth organic film layer.

[0029] Example 1

[0030] (1) Base film installation: using 125 micron thick polyester film (PET) pre-grown with 180 nm oxide film, and installing on the unwinding roller.

[0031] (2) Vacuum chamber vacuum pumping: starting automatic pumping of the film plating equipment, and the base vacuum is better than 3x10 -3 Pa.

[0032] (3) Ion source pretreatment: start winding, start the device anode layer ion source, pretreatment of the surface to be plated, adjust the surface wetting tension between 44-46 dynes.

[0033] (4) Plating polyacrylate film layer: using methyl acrylate, liquid flow meter control 1 ml / min flow, evaporator temperature 150°C.

[0034] (5) UV lamp curing, power is 600W, vacuum degree control in 1-2 Pa, base film winding speed 200 mm / min.

[0035] (6) Surface flatness test: after plating, using AFM test, as shown in Figure 1 , the surface roughness is less than 3 nm.

[0036] Example 2

[0037] (1) Base film installation: using 23 micron thick polyester film (PET), pre-grown with 60 nm oxide film, installed on the unwinding roller.

[0038] (2) Vacuum chamber vacuum: start plating equipment automatic pumping, the background vacuum is better than 3x10 -3 Pa.

[0039] (3) Ion source pretreatment: start winding, start the device anode layer ion source, pretreatment of the surface to be plated, adjust the surface wetting tension between 54-56 dynes.

[0040] (4) Plating polyacrylate film layer: using methyl acrylate, liquid flow meter control 3 ml / min flow, evaporator temperature 200°C.

[0041] (5) UV lamp curing, power is 800W, vacuum degree control in 1-2 Pa, base film winding speed 500 mm / min.

[0042] (6) Surface flatness test: after plating, using AFM test, the surface roughness is less than 3 nm.

[0043] Example 3

[0044] (1) Base film installation: using 50 micron thick polyester film (PET), pre-grown with 100 nm oxide film, installed on the unwinding roller.

[0045] (2) Vacuum chamber vacuum: start plating equipment automatic pumping, the background vacuum is better than 3x10 -3 Pa.

[0046] (3) Ion source pretreatment: start winding, start the device anode layer ion source, pretreatment of the surface to be plated, adjust the surface wetting tension between 48-50 dynes.

[0047] (4) Plating polyacrylate film layer: using methyl acrylate, liquid flow meter control 5 ml / min flow, evaporator temperature 250°C.

[0048] (5) UV lamp curing, power is 1000W, vacuum degree control in 1~2Pa, base film winding speed 400mm / min.

[0049] (6) Surface flatness test: after plating film, using AFM test, surface roughness less than 3nm.

Claims

1. A method for preparing an ultra-smooth organic film layer, characterized in that... The steps are as follows: The first step is to grow an oxide film on a polyester film to obtain the film to be coated, and then mount the film to be coated on the unwinding roller of a roll-to-roll vacuum evaporation coating machine. The second step is to evacuate the roll-to-roll vacuum evaporation coating machine that was installed with the coating to be coated in the first step. The third step is to start the winding of the roll-to-roll vacuum evaporation coating machine, turn on the ion source of the anode layer, and perform surface tension pretreatment on the surface to be coated. The fourth step is to deposit a polyacrylate film layer on the surface of the film to be coated obtained in the third step. The fifth step involves curing the product obtained in the fourth step with ultraviolet light and then winding the base film to obtain an ultra-smooth organic film layer. In the third step, when performing surface tension pretreatment on the surface to be coated, the wetting tension of the surface to be coated is made to be 44~56 dynes. In the fourth step, methyl acrylate is used when depositing the polyacrylate film, the flow rate is controlled by a liquid flow meter at 0.5~5 ml / min, and the evaporator temperature is 150~300℃.

2. The method for preparing an ultra-smooth organic film layer according to claim 1, characterized in that: In the first step, the thickness of the polyester film is 12-125 micrometers, and the thickness of the oxide film is 60-180 nm.

3. The method for preparing an ultra-smooth organic film layer according to claim 1 or 2, characterized in that: In the second step, the vacuum level of the roll-to-roll vacuum evaporation coating machine is made better than 3×10⁻⁶ during the evaporation process. -3 Pa.

4. The method for preparing an ultra-smooth organic film layer according to claim 1, characterized in that: In the fifth step, the power of the UV lamp during curing is 200~1000W, and the vacuum degree during UV lamp curing is 1~2Pa.

5. The method for preparing an ultra-smooth organic film layer according to claim 1, characterized in that: In the fifth step, the base film winding speed is 50~500mm / min.

6. The method for preparing an ultra-smooth organic film layer according to claim 1, characterized in that: The coating process using a roll-to-roll vacuum evaporation coating machine includes organic flash evaporation, organic flow leveling, and organic film polymerization.

7. The method for preparing an ultra-smooth organic film layer according to claim 1, characterized in that: The oxide film is a silicon oxide inorganic film or an aluminum oxide inorganic film.

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