Method for preparing a barrier film

Patent metadata

Field	Value
Publication number	US-10654070-B2
Application number	US-201715750815-A
Country	US
Kind code	B2
Filing date	Mar 31, 2017
Priority date	Mar 31, 2016
Publication date	May 19, 2020
Grant date	May 19, 2020

Abstract

The present application relates to a method for preparing a barrier film. The present application can provide a method for preparing a barrier film having excellent barrier characteristics and optical performances. The barrier film produced by the method of the present application can be effectively used not only for packaging materials of as foods or medicines, and the like, but also for various applications, such as members for FPDs (flat panel displays) such as LCDs (Liquid Crystal Displays) or solar cells, substrates for electronic papers or OLEDs (Organic Light Emitting Diodes), or sealing films.

First claim

The invention claimed is:

1. A method for preparing a water vapor transmission barrier film, the method comprising:
coating a composition comprising an amine catalyst and a polysilazane on a base layer via a wet coating process to form a barrier layer, wherein:
the amine catalyst is ammonia, ammonium hydroxide, ammonium chloride, trialkylamine, dialkylamine, monoalkyl amine, dialkanolamine, dialkylalkanolamine, trialkanolamine or dialkylaminoalkyl trialkoxysilane; and
the amine catalyst is present in an amount within a range of 0.1 to 10 parts by weight relative to 100 parts by weight of the polysilazane; and

subjecting the barrier layer to a curing process that includes performing a plasma hardening treatment comprising plasma-treating a surface of the barrier layer containing the polysilazane and the amine catalyst in a processing space in which water vapor, a discharge gas, and oxygen as a reaction gas are injected resulting in maintaining a vapor pressure of water vapor in the processing space at about 5% or more to cause oxidation of the polysilazane whereby SiN units of the polysilazane are converted into Si—O units in a thickness direction to layer satisfy Equation 2 below thereby yielding the water vapor transmission barrier film:
0.75 ≤d /( c+d )≤0.97  [Equation 2]

wherein:
c is the number of Si—N units present in the barrier layer after the plasma hardening treatment, and
d is the number of Si—O units present in the barrier layer after the plasma hardening treatment.

2. The method according to claim 1 , wherein the polysilazane has a repeating unit of Formula 1:

wherein each of R 1 , R 2 and R 3 separately is hydrogen, an alkyl group, an alkenyl group, an aryl group, a carbonyl group, a hydroxyl group or an alkoxy group.

3. The method according to claim 2 , wherein R 1 to R 3 in the repeating unit of the Formula 1 are hydrogen atoms.

4. The method according to claim 1 , wherein the polysilazane is present in an amount of 55 wt % or more.

5. The method according to claim 1 , wherein the plasma-treating is carried out while maintaining a hydrogen partial pressure in the processing space at 2.00×10 −5 Pa or more.

6. The method according to claim 1 , wherein a ratio (H/A) of an injection volumetric flow rate (H) of the water vapor to an injection volumetric flow rate (A) of the discharge gas is maintained at 0.4 or more.

7. The method according to claim 1 , wherein a ratio (H/O) of an injection volumetric flow rate (H) of the water vapor to an injection volumetric flow rate (O) of the oxygen is maintained at 0.4 or more.

8. The method according to claim 1 , wherein a process pressure during the plasma-treating is maintained at 50 mTorr or more.

9. The method according to claim 1 , wherein a power density during the plasma-treating is maintained at 0.2 W/cm 2 or more.

10. The method according to claim 1 , wherein a process energy density during the plasma-treating is maintained at 2 J/cm 2 or more.

11. The method according to claim 1 , wherein the water vapor transmission barrier film further comprises an undercoating layer between the base layer and the barrier layer.

Assignees

• Lg Chemical Ltd

Inventors

• Yang Hee Wang
• Hwang Jang Yeon
• Lee Seong Hwan

Classifications

• B32B27/34

  comprising polyamides · CPC title

• B32B27/36

  comprising polyesters · CPC title

• B32B2457/12

  Photovoltaic modules · CPC title

• C08J2483/16

  in which all the silicon atoms are connected by linkages other than oxygen atoms · CPC title

• B32B2439/80

  Medical packaging · CPC title