BARRIER FILM
20210387855 · 2021-12-16
Inventors
- Sung Jin Shin (Daejeon, KR)
- Jang Yeon Hwang (Daejeon, KR)
- Hee Joon Jeong (Daejeon, KR)
- Bo Ra Park (Daejeon, KR)
- Hee Wang Yang (Daejeon, KR)
Cpc classification
C08J2383/16
CHEMISTRY; METALLURGY
C09D183/16
CHEMISTRY; METALLURGY
C23C18/125
CHEMISTRY; METALLURGY
C08J7/06
CHEMISTRY; METALLURGY
C23C18/122
CHEMISTRY; METALLURGY
C08J2383/14
CHEMISTRY; METALLURGY
C08J7/042
CHEMISTRY; METALLURGY
C08J7/0427
CHEMISTRY; METALLURGY
International classification
Abstract
Provided is a barrier film, comprising: a base layer; and an inorganic layer including Si, N, and O, wherein the inorganic layer has a thickness of 600 nm or less, and the film has a water vapor transmission rate of 0.5×10.sup.−3 g/m.sup.2.Math.day as measured under conditions of a temperature of 38° C. and 100% relative humidity. The barrier film has excellent barrier properties and optical properties and can be used for electronic products sensitive to moisture.
Claims
1. A barrier film, comprising: a base layer; and an inorganic layer including Si, N, and O, wherein the inorganic layer has a thickness of 600 nm or less, and the film has a water vapor transmission rate of 0.5×10.sup.−3 g/m.sup.2.Math.day or less as measured under conditions of a temperature of 38° C. and 100% relative humidity.
2. The barrier film according to claim 1, wherein the inorganic layer has a thickness of 300 nm or less, and the water vapor transmission rate measured under conditions of a temperature of 38° C. and 100% relative humidity is 0.1×10.sup.−3 g/m.sup.2.Math.day or less.
3. The barrier film according to claim 2, wherein the inorganic layer has a compactness expressed through an etching rate of 0.17 nm/s or less in the thickness direction for an Ar ion etching condition to etch Ta.sub.2O.sub.5 at a rate of 0.09 nm/s.
4. The barrier film according to claim 3, wherein the inorganic layer comprises a first region and a second region, which have different elemental contents (atomic %) of Si, N, and O from each other as measured by XPS, and the first region is in a position closer to the base layer than the second region.
5. The barrier film according to claim 4, wherein the first region satisfies the relationship: O content>Si content>N content.
6. The barrier film according to claim 5, wherein the O content of the first region is in a range of 50 to 65 atomic %, the Si content of the first region is in a range of 35 to 45 atomic %, and the N content of the first region is in a range of 1 to 15 atomic %.
7. The barrier film according to claim 6, wherein the first region has a ratio (a/b) of the O content (a) to the Si content (b) in a range of 1.1 to 1.9.
8. The barrier film according to claim 6, wherein the second region satisfies the relationship: Si content>N content>O content.
9. The barrier film according to claim 8, wherein the Si content of the second region is in a range of 45 to 60 atomic %, the N content of the second region is in a range of 20 to 35 atomic %, and the O content of the second region is in a range of 10 to 30 atomic %.
10. The barrier film according to claim 9, wherein the N content in the second region is greater than the N content in the first region.
11. The barrier film according to claim 9, wherein the difference between the highest value of the Si content in the second region and the highest value of the O content in the first region is 15 atomic % or less.
12. The barrier film according to claim 1, wherein the inorganic layer is obtained by plasma-treating polysilazane having a unit of Formula 1 below: ##STR00003## wherein, R.sup.1, R.sup.2 and R.sup.3 are each independently a hydrogen atom, an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkylsilyl group, an alkylamino group or an alkoxy group.
13. An electrical or electronic element comprising the barrier film according to claim 1.
Description
BRIEF DESCRIPTION OF DRAWINGS
[0103]
[0104]
EXAMPLES
[0105] Hereinafter, the barrier film of the present application will be described through examples according to the present application and comparative examples, but the scope of the present application is not limited by the following examples.
[0106] Measuring Method [0107] Water vapor transmission rate: Using MOCON Aquatron II, the water vapor transmission rate of the produced barrier film was measured at 38° C. and 100% relative humidity conditions. [0108] Etching rate and elemental content analysis: The element distribution analysis in the depth (thickness) direction from the surface of the inorganic material layer to the base material direction was performed while gradually removing the inorganic layer using Ar ions. As the etching conditions, an Ar ion setting with an etching rate of 0.09 nm/s for Ta.sub.2O.sub.5 as the reference material was used. In addition, the elemental contents of the inorganic layer were analyzed using XPS (X-ray photoelectron spectroscopy) (C can be detected as an impurity derived from the base material).
[0109] The thickness, etching rate, and water vapor transmission rate of the barrier film produced as described below were measured, and the results were described in Table 1.
Example 1
[0110] A planarizing layer having a thickness of 1 μm was laminated on a PET (poly(ethylene terephthalate)) film (a product from Teijin Co., Ltd.) having a thickness of about 50 μm, and an inorganic material layer was formed on the planarizing layer. The specific process is as follows.
[0111] Formation of planarizing layer: A composition comprising 2 ratios by weight of a photocuring initiator to a mixture of fluorine-based acrylate HR6060:PETA (pentaerythritol triacrylate):DPHA (dipentaerythritol hexaacrylate) in a content (weight) ratio of 80:10:10 was diluted in PGME (propylene glycol methyl ether) to 25% to prepare a coating liquid for a planarizing layer. The coating liquid was applied onto a PET film as a base material using a Mayer bar, and dried at 100° C. for 5 minutes. Subsequently, the coating layer was irradiated with ultraviolet rays at 0.6 J/cm.sup.2 by a mercury lamp, and cured to form a planarizing layer. 10 different regions having an area of about 100 μm.sup.2 of the surface of the planarizing layer were designated, and the height difference between the highest part and the lowest part in each region was obtained by using Optical Profiler, and an average surface roughness value (Rt) of 34 nm (standard deviation 5.8 nm) was obtained.
[0112] Formation of inorganic coating layer (1): Polysilazane was diluted to 3.7% with Merck's NL grade dibutylether, coated on the planarizing layer using a Mayer bar, and then dried at 100° C. for 5 minutes. A plasma treatment was performed on the polysilazane coating layer under the following conditions, and an inorganic coating layer was formed. Regarding the concentration of the diluted polysilazane, % means the weight ratio of the total solid content. [0113] Pressure 250 mTorr (flow rate on the basis of sccm atmosphere of Ar:O.sub.2:H.sub.2O=1.5:1:1) [0114] Distance between polysilazane coated surface and electrode 25 mm [0115] Power density: supply of DC power 0.8 W/cm.sup.2 for 25 seconds
[0116] Formation of inorganic coating layer (2): On the inorganic coating layer (1), a polysilazane layer was further formed by using a coating liquid having a silazane concentration of 3.7%, and the plasma treatment was performed under the same conditions as in Example 1 to further form an inorganic coating layer (2).
Example 2
[0117] An inorganic coating layer (1-1) replacing the inorganic layer (1) of Example 1 was formed under the same conditions using a coating liquid having a silazane concentration of 1.1%. The other configurations are the same as in Example 1.
Example 3
[0118] On the inorganic coating layer (1) manufactured in Example 1, a polysilazane layer was further formed by using a coating liquid having a silazane concentration of 1%, and the plasma treatment was performed under the same conditions as in Example 1 to further laminate an inorganic coating layer (2).
Comparative Example 1
[0119] A barrier film was produced in the same manner as in Example 1, except that the polysilazane solution diluted to 4.5% was used and the plasma conditions were changed as follows. [0120] Pressure 100 mTorr (flow rate on the basis of sccm atmosphere of Ar:O.sub.2=1:1) [0121] Distance between polysilazane coated surface and electrode 10 mm [0122] Power density: supply of DC power 0.3 W/cm.sup.2 for 65 seconds
Comparative Example 2
[0123] A barrier film was produced in the same method as in Comparative Example 1, except that the polysilazane solution diluted to 4.9% was used and the distance from the electrode was 175 mm.
TABLE-US-00001 TABLE 1 Inorganic layer Water vapor Etching Etching transmission Thickness time rate rate (nm) (s) (nm/s) (×10.sup.−3 g/m.sup.2 .Math. day) Example 1 250 1,600 0.156 <0.05 2 150 950 0.158 0.08 3 185 1,180 0.157 <0.05 Comparative 1 180 700 0.257 2.39 Example 2 200 760 0.263 1.20
[0124] As in Table 1, it can be seen that Examples comprising the inorganic layer satisfying an etching rate of 0.17 nm/s or less have very low water vapor transmission rates relative to Comparative Examples which do not satisfy the etching rate. In particular, in can be confirmed that in the case of Example 2 of the present application, the thickness of the inorganic layer is thinner than those of Comparative Examples, but the excellent water vapor transmission rate can be ensured. This means that the inorganic layers of the barrier films in Examples are denser than the inorganic layers of the barrier films in Comparative Examples.
[0125] On the other hand, the silazane solution of 4.8% in total was used upon producing the barrier film of Example 2, and the silazane solution of 4.9% in total was used upon producing the barrier film of Comparative Example 2, whereby the concentrations of the silazane solutions were almost similar (the concentration of Comparative Example was higher), but it can be seen that the difference in water vapor transmission rate occurred. This suggests that the compactness of the film is not due to the concentration of the coating solution.