A method for preparing an organic film layer on a silicone surface

Abstract

The application provides a method for preparing an organic film layer on a siloxane surface, and relates to the field of electronic product packaging. The method for preparing an organic film layer on a siloxane surface comprises the following steps: ion source activation is performed on the surface of the siloxane; a substrate wetting agent is mixed into an acrylate solution to obtain a coating material; the coating material is used to grow an acrylate organic film layer on the surface of the siloxane after ion source activation by means of vacuum evaporation; and the organic film layer is subjected to ultraviolet curing. In one aspect, the surface energy of the siloxane surface is improved by ion source activation, and in another aspect, a surface wetting agent is added to the organic liquid, so that the organic liquid can fully infiltrate the surface of the siloxane. The method of vacuum evaporation is used to grow an organic film layer on the surface of the siloxane. The method solves the problem that the low surface energy of the siloxane film surface leads to the inability of the organic matter to form a film layer, realizes continuous winding deposition of the organic film layer in a vacuum environment, and realizes the development of an ultrahigh barrier film product.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of electronic product packaging, in particular to a method for preparing an organic film layer on a silicone surface. BACKGROUND

[0002] In order to achieve the long service life of flexible electronic products and ensure the core functions thereof from being eroded by water vapor and oxygen, the barrier ability of the packaging material thereof must reach the index level of 10 -3 (unit g / (m 2 ·day) or above, even 10 -6 The mainstream technical route for preparing the packaging material of the water vapor and oxygen barrier film with ultra-high index is an organic / inorganic lamination scheme, and the typical structure of the barrier film lamination is 50-100 μm PET / organic layer / inorganic barrier layer / organic layer, wherein the inorganic layer has high barrier performance, and the organic layer can flatten the base film and fill the defects such as pinholes and micro-cracks of the inorganic layer.

[0003] A typical inorganic film layer is a silicone film layer, which has high barrier performance and certain flexibility. However, the surface energy of the silicone film surface is low, generally less than 40 dynes, and when the organic film layer is deposited to form a liquid film, it cannot be infiltrated, small droplets visible to the naked eye are generated, and a complete organic film layer cannot be formed. Precision coating is a commonly used organic film layer preparation technology in industrial production, which mainly uniformly coats the formula liquid on the surface of the substrate, and then dries or solidifies to form a stable coating. However, due to the precision of the spraying unit and the heat shrinkage in the solidification process, whether the coating liquid is water-based or solvent-based, the thickness of the film layer is reduced to 10%-30% of the original during the solidification process. Defects such as thermal wrinkles are inevitable in the solidification process, and uneven coating on the surface, i.e. "orange peel", "stripes", and other phenomena are easily generated.

[0004] How to solve the problems of the inability of the organic matter to form a complete film layer and the uneven formation of the film layer due to the low surface energy of the silicone film surface has become a technical problem to be solved by the technical personnel in the field. SUMMARY

[0005] Therefore, the technical problem to be solved by the present application is to overcome the defect that it is difficult to form a uniform and complete organic film layer on the surface of the silicone in the prior art, so as to provide a method for preparing an organic film layer on a silicone surface.

[0006] To achieve the above-mentioned purpose, the present application provides the following technical scheme:

[0007] The present application provides a method for preparing an organic film layer on a silicone surface, comprising the following steps:

[0008] (1) ion source activation is performed on the surface of the silicone;

[0009] (2) mixing a substrate wetting agent into the acrylate solution to obtain a coating material;

[0010] (3) using the coating material, growing an acrylate organic film layer on the ion source activated silicone surface by vacuum evaporation;

[0011] (4) ultraviolet curing the organic film layer.

[0012] Further, in step (1), the ion source activation conditions include: base vacuum 3×10 -3 Pa, using an anode layer ion source, current density 5-10 mW / cm 2 .

[0013] Further, in step (1), the surface energy of the ion source activated silicone surface is 40-50 dynes.

[0014] Further, in step (2), the substrate wetting agent is Tego Wet 280 substrate wetting agent.

[0015] Further, in step (2), the volume of the substrate wetting agent is 1%-3% of the acrylate solution.

[0016] Further, in step (2), the surface energy of the coating material is 30-40 dynes.

[0017] Further, in step (3), the vacuum evaporation conditions: base vacuum less than 3×10 -3 Pa before coating, vacuum chamber vacuum pressure 1-10 Pa during evaporation.

[0018] Further, in step (4), the ultraviolet curing conditions: using a 395 nm LED ultraviolet lamp, power 1-10 w / cm 2 .

[0019] Further, using a roll-to-roll vacuum coating equipment to prepare an organic film layer on the silicone surface, the winding speed is 1-10 m / min, and the coating material flow during coating is 0.1-10 mL / min.

[0020] Further, the surface energy of the silicone surface is 30-34 dynes.

[0021] Further, the thickness of the organic film layer is 0.2-3 μm.

[0022] The technical scheme of the present application has the following advantages:

[0023] The present application improves the surface energy of the silicone surface by ion source activation, and adds surface wetting agent to the organic liquid, so that the organic liquid can fully infiltrate the silicone surface. The organic film layer is grown on the silicone surface by vacuum evaporation method. The problem that the organic matter cannot form a film layer due to the low surface energy of the silicone film surface is solved, the continuous winding deposition of the organic film layer in vacuum environment is realized, and the development of ultra-high barrier film product is realized. DETAILED DESCRIPTION

[0024] The following examples are provided to better further understand the present application, and are not limited to the best mode, and do not limit the content and protection scope of the present application. Any product which is the same or similar to the present application obtained by the inspiration of the present application or the combination of the present application with other prior art features falls within the protection scope of the present application.

[0025] The acrylate solution uses non-irritating TPGDA (tripropylene glycol diacrylate) monomer solution, and the vacuum evaporation equipment uses 600mm width roll-to-roll vacuum coating equipment.

[0026] If the specific experimental steps or conditions are not specified in the examples, the operation or conditions can be carried out according to the conventional experimental steps described in the literature in the art. The raw materials or instruments used are conventional products that can be obtained by purchase, including but not limited to the raw materials or instruments used in the examples of the present application.

[0027] Example 1

[0028] The present example provides a method for preparing an organic film layer on a silicone surface, and the specific operation is as follows:

[0029] (1) For a silicone substrate with a surface energy of 30 dynes, ion source activation is first performed, and the base vacuum is 3x10 -3 Pa, the winding speed is 1m / min, the anode layer ion source is used, the current density is 10mW / cm 2 , and the surface energy of the silicone surface after ion source activation is 40 dynes;

[0030] (2) 1% Wet 280 substrate wetting agent is mixed into the acrylate solution to obtain a coating material with a surface energy of 30 dynes;

[0031] (3) The coating material is used to grow an acrylate organic film layer on the ion source activated silicone surface by vacuum evaporation method, the winding speed is 1m / min, the coating material flow is 0.1mL / min, the vacuum pressure is controlled at 1-3Pa, the organic matter is uniformly spread on the silicone surface, and the organic film layer is formed;

[0032] (4) Using 395 nm wavelength ultraviolet lamp to cure the organic film layer, power 8 w / cm 2 , forming film layer surface roughness <10 nm.

[0033] Example 2

[0034] This embodiment provides a method for preparing an organic film layer on a silicone surface, the specific operation as follows:

[0035] (1) For a silicone substrate with a surface energy of 30 dynes, first ion source activation, base vacuum 3 x 10 -3 Pa, winding speed 1 m / min, using anode layer ion source, current density 5 mW / cm 2 , the surface energy of the silicone surface after ion source activation is 40 dynes;

[0036] (2) Mix 1% Wet 280 substrate wetting agent into the acrylate solution to obtain a coating material with a surface energy of 30 dynes;

[0037] (3) Using the coating material, grow an acrylate organic film layer on the ion source activated silicone surface by vacuum evaporation, winding speed 5 m / min, coating material flow 0.5 mL / min, vacuum pressure controlled at 4-8 Pa, organic matter evenly spread on the silicone surface, forming an organic film layer;

[0038] (4) Using 395 nm wavelength ultraviolet lamp to cure the organic film layer, power 8 w / cm 2 , forming film layer surface roughness <10 nm.

[0039] Example 3

[0040] This embodiment provides a method for preparing an organic film layer on a silicone surface, the specific operation as follows:

[0041] (1) For a silicone substrate with a surface energy of 32 dynes, first ion source activation, base vacuum 3 x 10 -3 Pa, winding speed 3 m / min, using anode layer ion source, current density 5 mW / cm 2 , the surface energy of the silicone surface after ion source activation is 40 dynes;

[0042] (2) Mix 2% Wet 280 substrate wetting agent into the acrylate solution to obtain a coating material with a surface energy of 36 dynes;

[0043] ​​(3) using the coating material, the vacuum evaporation method is used to grow the acrylate organic film layer on the siloxane surface after ion source activation, the winding speed is 1 m / min, the coating material flow is 0.1 mL / min, the vacuum pressure is controlled at 2-4 Pa, the organic matter is uniformly spread on the siloxane surface, and the organic film layer is formed;

[0044] (4) using a 395 nm wavelength ultraviolet lamp to ultraviolet cure the organic film layer, the power is 4 w / cm 2 , the surface roughness of the film layer is less than 10 nm.

[0045] Example 4

[0046] The embodiment provides a method for preparing an organic film layer on a siloxane surface, and the specific operation is as follows:

[0047] (1) for a siloxane substrate with a surface energy of 34 dynes, ion source activation is first performed, the background vacuum is 3*10 -3 Pa, the winding speed is 5 m / min, the anode layer ion source is used, the current density is 5 mW / cm 2 , and the surface energy of the siloxane surface after ion source activation is 50 dynes;

[0048] (2) 2% of Wet 280 substrate wetting agent is mixed into the acrylate solution to obtain a coating material with a surface energy of 36 dynes;

[0049] (3) using the coating material, the vacuum evaporation method is used to grow the acrylate organic film layer on the siloxane surface after ion source activation, the winding speed is 5 m / min, the coating material flow is 5 mL / min, the vacuum pressure is controlled at 6-10 Pa, the organic matter is uniformly spread on the siloxane surface, and the organic film layer is formed;

[0050] (4) using a 395 nm wavelength ultraviolet lamp to ultraviolet cure the organic film layer, the power is 10 w / cm 2 , the surface roughness of the film layer is less than 10 nm.

[0051] Example 5

[0052] The embodiment provides a method for preparing an organic film layer on a siloxane surface, and the specific operation is as follows:

[0053] (1) for a siloxane substrate with a surface energy of 34 dynes, ion source activation is first performed, the background vacuum is 3*10 -3 Pa, the winding speed is 10 m / min, the anode layer ion source is used, the current density is 5 mW / cm 2 , and the surface energy of the siloxane surface after ion source activation is 50 dynes;

[0054] (2) 3% of Wet 280 substrate wetting agent is mixed into the acrylate solution to obtain a coating material with a surface energy of 36 dynes; ​Wet 280 substrate wetting agent, to obtain a coated material, surface energy 40 dynes;

[0055] (3) using the coated material, using vacuum evaporation to grow an acrylate organic film layer on the activated siloxane surface, winding speed 10 m / min, coated material flow 10 mL / min, vacuum pressure controlled at 8-10 Pa, organic matter evenly spread on the siloxane surface, forming an organic film layer;

[0056] (4) using a 395 nm wavelength ultraviolet lamp to cure the organic film layer, power 10 w / cm 2 , forming a film layer surface roughness <10 nm.

[0057] Comparative Example

[0058] The present comparative example provides a method for preparing an organic film layer on a siloxane surface, the specific operation refers to Example 1, the difference is only in step (2), the acrylate solution does not mix Wet 280 substrate wetting agent, by testing the surface roughness of the formed film layer, the roughness is more than 10 nm.

[0059] While in the example, the acrylate solution is mixed with Wet 280 substrate wetting agent, the siloxane component contained in the substrate wetting agent helps the liquid film to spread, prevents the formation of liquid small particles, and helps to reduce the roughness of the organic film layer, and finally forms a film layer surface roughness less than 10 nm.

[0060] Obviously, the above examples are only examples for the purpose of clarity, and are not limitations of the embodiments. For those skilled in the art, other different forms of changes or variations can also be made on the basis of the above description. Here, it is not necessary and impossible to exhaust all the embodiments. The obvious changes or variations derived therefrom are still within the protection scope of the present invention.

Claims

1. A method for producing an organic film layer on a silicone surface, characterized by, The method comprises the following steps: (1) ion source activation on the surface of the silicone; (2) mixing a substrate wetting agent into the acrylate solution to obtain a coating material; (3) growing an acrylate organic film layer on the ion source activated surface of the silicone by vacuum evaporation using the coating material; (4) ultraviolet curing the organic film layer, wherein In step (1), the ion source activation conditions include: base vacuum 3x10 -3 Pa, using an anode layer ion source, current density 5~10 mW / cm 2 After ion source activation, the surface energy of the siloxane surface is 40~50 dynes, In step (2), the substrate wetting agent is Tego Wet 280 substrate wetting agent, the volume of the substrate wetting agent is 1-3% of the volume of the acrylate solution, and the surface energy of the coating material is 30-40 dynes.

2. The method of claim 1, wherein the method is characterized by: In step (3), the winding speed is 1-10 m / min, the plating material flow is 0.1-10 mL / min, and the vacuum evaporation conditions are as follows: the base vacuum before plating is less than 3×10 -3 Pa, and the vacuum chamber pressure during evaporation is 1-10 Pa.

3. The method of claim 1, wherein the method is characterized by: In step (4), the condition of UV curing: using 395 nm LED UV lamp, power 1~10 w / cm 2 .

4. The method of claim 1, wherein the method is characterized by: The surface energy of the surface of the silicone is 30-34 dynes.

5. The method of claim 1, wherein the method is characterized by: The thickness of the organic film layer is 0.2-3 microns.