KR101715688B1 - Release films and methods of manufacturing the same - Google Patents

Release films and methods of manufacturing the same Download PDF

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Publication number
KR101715688B1
KR101715688B1 KR1020160010088A KR20160010088A KR101715688B1 KR 101715688 B1 KR101715688 B1 KR 101715688B1 KR 1020160010088 A KR1020160010088 A KR 1020160010088A KR 20160010088 A KR20160010088 A KR 20160010088A KR 101715688 B1 KR101715688 B1 KR 101715688B1
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South Korea
Prior art keywords
release
metal oxide
oxide particles
weight
release layer
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KR1020160010088A
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Korean (ko)
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황보격
정진국
이성규
김범호
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율촌화학 주식회사
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    • C09J7/0228
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • C09J7/0285
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Laminated Bodies (AREA)

Abstract

A release film formed on a base film, the release layer comprising a release layer comprising a solventless silicone release agent and metal oxide particles, wherein the release layer has an average thickness of 0.07 to 2 m, and the metal oxide particles have an average diameter of 2 to 5 m Wherein the average particle diameter of the metal oxide particles is larger than the average thickness of the release layer.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a release film,

The present invention relates to a release film having excellent physical properties and a method for producing the same. More particularly, the present invention relates to a release film having excellent adhesion, residual adhesion, and the like, and a method for producing the same.

In general, release films are mainly used for protection of the pressure-sensitive adhesive layer, and these release films are widely used in general industrial adhesive (or adhesive) tapes and the like. In recent years, they have been widely used in mobile phones, LCDs, semiconductors, And so on.

On the other hand, the release film generally comprises a base film and a release layer formed on the base film. A base film or a plastic film is often used as the base film, and the release layer is mainly a siloxane-based silicone composition. The silicone composition is divided into a solvent type and a non-solvent type. In the solvent type, it is easy to adjust the releasing force, but a large amount of organic solvent must be diluted in order to adjust the viscosity of the releasing agent having a high viscosity (5000mpa.s or more) This causes problems.

Currently, European countries are limiting the use of solvent-based silicone release agents and related product imports due to the emission of environmentally harmful substances. As a result, a silicone-free silicone-free type having a relatively low volatile organic compound emission has attracted attention.

However, since the solventless silicone release agent has limited dilution ratio with the organic solvent and has difficulty in adjusting the coating thickness of the substrate surface, it has been applied only to the release paper industry in which a release agent is coated on a paper substrate using a comma coating system.

Accordingly, there is a demand for the development of a releasing film for adhesive protection that protects the pressure-sensitive adhesive layer stably and has a higher speed stability than a case of using a solvent-type silicone release agent and realizes releasing force in a low region.

KR 10-2001-0087777 A1

Embodiments of the present invention provide a release film having excellent physical properties and a method for producing the same.

Other embodiments of the present invention are intended to provide a release film having excellent adhesion, residual adhesion, etc., and a method for producing the same.

In one embodiment of the invention, a substrate film; And a release layer formed on the base film, wherein the release layer comprises a solventless silicone release agent and metal oxide particles, wherein the release layer has an average thickness of 0.07 to 2 mu m, and the metal oxide particles have a thickness of 2 to 5 mu m And the average particle diameter of the metal oxide particles is larger than the average thickness of the release layer.

In an exemplary embodiment, the metal oxide particles may be metal oxide beads.

In an exemplary embodiment, the substrate film may be a corona discharge treated polyester film.

In an exemplary embodiment, the solventless silicone release agent and the metal oxide particles may be mixed in the release layer at a ratio of 30 to 50: 0.1 to 2 parts by weight, respectively.

In an exemplary embodiment, the solventless silicone release agent may have a viscosity of from 200 to 1,000 mPa.s at 25 [deg.] C.

In an exemplary embodiment, the solventless silicone release agent may have a weight average molecular weight of 10,000 to 20,000.

In an exemplary embodiment, the metal oxide particles may include at least one selected from the group consisting of silica, titanium dioxide (TiO 2 ), aluminum oxide (Al 2 O 3 ), and zinc dioxide (ZnO 2 ).

In an exemplary embodiment, the solventless silicone release agent may be a siloxane-based release agent.

In another embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: applying a release composition comprising a silicone release agent, metal oxide particles, a metal catalyst and a solvent on a substrate film; And drying the releasing composition to form a release layer; Wherein the metal oxide particles have an average particle diameter of from 2 to 5 mu m and an average particle diameter of the metal oxide particles is greater than an average thickness of the release layer, and the release layer has a thickness of 0.07 to 2 mu m, A method for producing a film is provided.

In an exemplary embodiment, the mold release composition comprises 30 to 50 parts by weight of a silicone release agent, 0.1 to 2 parts by weight of a metal oxide particle, 5 to 10 parts by weight of a metal catalyst, and 30 to 50 parts by weight of a solvent, based on 100 parts by weight of the mold- .

In an exemplary embodiment, the mold release composition may have a viscosity of from 50 to 100 MPa.s at 25 占 폚.

In an exemplary embodiment, the step of drying the releasing composition may be performed at a temperature of from 110 to 130 < 0 > C.

In an exemplary embodiment, the step of applying the mold release composition may be performed through a microgravure coating process.

A release film according to one embodiment of the present invention comprises a solventless silicone release agent and metal oxide particles. The solventless silicone release agent generally has low viscosity, releasing force and speed stability, including resins having a short chain chain length as compared with a solvent type silicone release agent. Accordingly, the release film is easy to control the thickness and can have a good releasing force.

Further, in the present invention, there is provided a release film comprising metal oxide particles having an average particle diameter larger than the thickness of the release layer. If the thickness of the release layer is larger than the average particle diameter of the metal oxide particles, the releasing force may be reduced by adhering to the interface between the pressure-sensitive adhesive layer and the release film. On the other hand, in the present invention, the average particle diameter of the metal oxide particles is larger than the thickness of the release layer, thereby reducing the surface area of the release layer adhering to the interface between the release layer and the release layer and minimizing the interaction between the release film and the release layer The releasing force can be maximized.

The present invention also provides an optimal content range of the solventless silicone release agent and metal oxide particles, an optimum thickness range of the release layer and an optimum average particle size range of the metal oxide particles within the release layer. Accordingly, it is possible to provide an excellent releasing film having excellent releasing force as compared with the conventional releasing film and maintaining excellent characteristics such as residual adhesive ratio.

1 is a cross-sectional view of a release film according to an embodiment of the present invention.
FIGS. 2A to 2C are scanning electron microscope (SEM) photographs of the surface state of the release film according to an embodiment of the present invention.
3A to 3C are SEM photographs showing surface states of metal oxide particles in the release film according to an embodiment of the present invention.
FIG. 4 is a graph showing a result of measurement of release force of a release film according to an embodiment of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is to be understood that the same is by way of illustration and example only and is not to be construed as limiting the scope of the present invention.

As used herein, the term " solvent-free silicone release agent " means a silicone release agent prepared so that the solvent contained in the coating material for producing the silicone release agent is not volatilized but is part of the silicone release agent.

In the present specification, the "average thickness of the release layer" refers to the average distance (h1) from the lowest surface of the release layer to the upper surface of the non-protrusion of the release layer and the distance h2 from the lowest surface of the release layer to the protrusion of the release layer .

Release film

In one embodiment of the invention, a substrate film; And a release layer formed on the base film, wherein the release layer comprises a solventless silicone release agent and metal oxide particles, wherein the release layer has an average thickness of 0.07 to 2 mu m, and the metal oxide particles have a thickness of 2 to 5 mu m And the average particle diameter of the metal oxide particles is larger than the average thickness of the release layer.

1 is a cross-sectional view showing a release film according to an embodiment of the present invention. Hereinafter, the release film will be described in detail with reference to FIG.

Referring to Figure 1, a release film 100 according to the present invention includes a base film 10 and a release layer 30 comprising a solventless silicone release agent (not shown) and metal oxide particles 20.

In an exemplary embodiment, the base film 10 is a support for the release layer, which may be a paper, a polyethylene naphthalate (PEN), a polybutylene terephthalate (PBT), a polyimide (PI), an unoriented polypropylene And stretched polypropylene (OPP).

In one embodiment, the substrate film 10 may be a polyethylene terephthalate film.

In one embodiment, the substrate film 10 may be a corona treated polyethylene terephthalate film, where strong chemical bonds may be formed between the substrate film 10 and the release layer 30.

In an exemplary embodiment, the substrate film 10 may be made to have a thickness of 10 to 200 [mu] m. When the base film 10 has a thickness of less than 10 탆, coating of the release layer described later may not be smooth. If the base film 10 has a thickness of more than 200 탆, additional costs may occur. Lt; / RTI >

On the other hand, the release layer 30 is a layer for protecting a target article to which the release film is used, and can be easily peeled off from the base film 10.

The release layer 30 may include a solventless silicone release agent and metal oxide particles 20. The average particle diameter R of the metal oxide particles 20 may be greater than the average thickness of the release layer 30 The region where the metal oxide particles 20 are provided may have a shape protruding from the release layer 30. [

Hereinafter, for convenience of explanation, the region where the metal oxide particle 20 is provided in the release layer 30 is expressed as a protrusion, and the region where the metal oxide particle 20 is not provided is represented as a non-protrusion (see FIG. 1) )

1, the thickness of the non-lead portion in the release layer 30 (i.e., the vertical distance h1 from the bottom surface to the top surface of the release layer in the region where the metal oxide particles are not provided, h1) And may have a value smaller than the average particle diameter (R). On the other hand, in the projecting portion of the release layer 30, a solventless silicone release agent can be formed so as to surround the upper portion of the metal oxide particles 20, so that the thickness of the projected portion in the release layer 30 The vertical distance h2 from the bottom surface to the top surface of the release layer in the region may have a value larger than the average particle diameter R of the metal oxide particles 20. [

Since the thickness of the non-derivatized portion of the release layer 30 is smaller than the average diameter R of the metal oxide particles 20, the release layer 30 may include a plurality of protrusions as a whole, Lt; / RTI >

Specifically, when the thickness of the release layer of the release film is larger than the average particle diameter of the metal oxide particles, the releasing force may be reduced at the interface between the release layer and the adhesive layer to which the release film is applied. In contrast, in the present invention, since the average particle diameter of the metal oxide particles 20 is formed to be larger than the thickness of the release layer 30, the surface area of the release layer adhered to each other at the interface between the release layer and the pressure- And the adhesive layer are minimized, so that the releasing force can be maximized.

In an exemplary embodiment, the release layer 30 may have an average thickness of 0.07 to 2 m. If the average thickness of the release layer 30 is less than 0.07 m, the release layer 30 may be excessively thin and the release force may not be realized sufficiently. If the average thickness exceeds 2 m, the average thickness of the release layer 30 Can be formed larger than the metal oxide particles 20, so that the physical function on the surface of the release film (i.e., minimization of the interaction between the adhesive layer and the release film) can be lost, and the manufacturing cost can be unnecessarily increased .

In an exemplary embodiment, the release layer 30 may comprise a solventless silicone release agent and metal oxide particles 20.

At this time, the solvent-free silicone release agent and the metal oxide particles 20 may be mixed in the release layer 30 at a ratio of 30 to 50: 0.1 to 2 parts by weight. If the solvent-free silicone release agent and the metal oxide particle are not in the above-mentioned ratio range, physical properties such as release force and residual adhesion ratio of the release film may not be excellent.

In an exemplary embodiment, the solventless silicone release agent may be a siloxane based release agent or the like.

In one embodiment, the solventless silicone release agent may comprise polydimethylsiloxane, polymethylphenylsiloxane, polydiphenylsiloxane, and the like.

The solventless silicone release agent generally includes a resin having a shorter chain chain length as a base resin than a solvent-type silicone release agent, and has a low viscosity, a releasing force and a speed stability. Accordingly, the releasing film including the releasing film can be easily adjusted in thickness and can have a good releasing force.

The silicone-free silicone release agent may have a weight-average molecular weight of 10,000 to 20,000, and when the silicone-free silicone release agent has a weight-average molecular weight within the above range, coating is easy and productivity in the production process of the release film is improved .

In an exemplary embodiment, the solventless silicone release agent may have a viscosity ranging from 200 to 1,000 mPa.s at 25 [deg.] C. When the solventless silicone release agent has a viscosity within the above range, the coating can be easily performed, and the productivity in the production process of the release film can be improved.

The metal oxide particles 20 are used in combination with the silicone-free release agent to improve releasing force of the release film. In the release layer 30, May have a shape protruding from the release layer (30).

In one embodiment, the metal oxide particles 20 may be metal oxide beads. That is, the metal oxide particles 20 may have a circular shape.

Meanwhile, the metal oxide particles 20 may include at least one selected from the group consisting of silica, titanium dioxide (TiO 2 ), aluminum oxide (Al 2 O 3 ), and zinc dioxide (ZnO 2 ).

In an exemplary embodiment, the metal oxide particles 20 may have an average particle size of from 2 to 5 [mu] m. When the average particle diameter of the metal oxide particles 20 is 2 占 퐉, the target releasing force may not be realized. When the average particle diameter of the metal oxide particles 20 exceeds 5 占 퐉, the coating thickness of the release layer 30 becomes excessively large And the production cost can be excessively increased.

The above-mentioned release film includes a release-type silicone release agent and a release layer in which metal oxide particles are mixed. As a result, not only a speed stability is achieved but a releasing force in a low region can be realized as compared with the case where a solvent type silicone release agent is used.

Particularly, in the present invention, since the average particle diameter of the metal oxide particles is formed to be larger than the thickness of the release layer, the surface area of the release layer adhered to the release layer at the interface between the release layer and the release layer is reduced, It is minimized and the releasing force can be maximized. Accordingly, the release film can be widely used in the field of industry in general.

Method for producing release film

In another embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: applying a release composition comprising a silicone release agent, metal oxide particles, a metal catalyst and a solvent on a substrate film; And drying the releasing composition to form a release layer; A method for producing a release film is provided.

Hereinafter, this will be described in detail.

First, a releasing composition comprising a solventless silicone release agent, metal oxide particles, a metal catalyst and a solvent is applied onto a substrate film.

In an exemplary embodiment, the mold release composition comprises, based on 100 parts by weight of the mold release composition, 30 to 50 parts by weight of a solventless silicone release agent, 0.1 to 2 parts by weight of metal oxide particles, 5 to 10 parts by weight of a metal catalyst, Parts by weight.

In an exemplary embodiment, if the mold release composition comprises less than 5 parts by weight of the metal catalyst, the degree of cure of the release layer formed may be reduced to degrade the quality of the product, and if it comprises more than 10 parts by weight of the metal catalyst The production cost of the product can be improved since it does not affect the degree of curing. In addition, when the mold release composition contains less than 30 parts by weight of solvent, the cohesive force of the solvent-free silicone release agent is lost and defects may occur in the release layer. When the solvent contains more than 50 parts by weight, It may be limited and cause a manufacturing inconvenience.

In one embodiment, the metal oxide particles can be made to have an average particle size (R) of 2 to 5 [mu] m.

And the solventless silicone release agent has a weight average molecular weight of 10,000 to 20,000 and a viscosity of 200 to 1,000 mpa.s.

Thereafter, the mold release composition can be dried to form a release layer. Thus, a release layer having an average thickness of 0.07 to 2 mu m can be produced. At this time, the average particle diameter of the metal oxide particles may be larger than the average thickness of the release layer, and thus the metal oxide particles may be formed to have a shape protruding from the release layer.

Thus, a release film comprising a release layer formed on a base film can be produced through the above-described method.

Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for illustrating the present invention and that the scope of the present invention is not construed as being limited by these embodiments.

Example

Example 1

After the polyester base film was subjected to corona discharge treatment, 25 parts by weight of a solvent-free silicone release agent (Shin-Etsu, KNS 1724, weight average molecular weight: 10,000 to 20,000, 0.1 part by weight of spherical silica beads having a particle size of 2 탆, 1.9 parts by weight of a Pt-based catalyst (Shin-Etsu), and 73 parts by weight of methyl ethyl ketone (MEK) were dispersed using a microgravure coater , And an average thickness of 1.5 μm. Thereafter, the composition was dried by hot air for 20 seconds at a temperature of 120 ° C. to form a release layer, thereby producing a release film comprising a release layer formed on the base film.

Example 2

In Example 1, the same steps as in Example 1 were carried out except that 0.3 parts by weight and 1.7 parts by weight of spherical silica beads and Pt catalysts each having an average particle diameter of 2 μm were contained in the releasing composition, 2 was prepared.

Example 3

A release film according to Example 3 was prepared in Example 1, except that 0.5 parts by weight of spherical silica beads having an average particle diameter of 2 占 퐉 was contained in the releasing composition.

Example 4

The procedure of Example 1 was repeated except that 1 part by weight and 2 parts by weight of a silica bead and a Pt-based catalyst each having an average particle diameter of 2 μm were contained in the mold-releasing composition, To prepare a release film.

Example 5

In Example 2, a release film according to Example 5 was prepared by performing the same process as in Example 2, except that the release layer was applied to have an average thickness of 1 m.

Example 6

In Example 2, a release film according to Example 6 was produced by carrying out the same process as in Example 2, except that the release layer was applied so as to have an average thickness of 2 탆.

The differences between the release films according to Examples 1 to 6 are shown in Table 1 below.

Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Silica bead content (parts by weight) 0.1 0.3 0.5 One 0.3 0.3 Composition average coating thickness
(μm)
1.5 1.5 1.5 1.5 One 2

Comparative Example  One

After the polyester base film was subjected to corona discharge treatment, 25 parts by weight of a solvent-free silicone release agent (Shin-Etsu, KNS 1724, weight average molecular weight: 10,000 to 20,000, Viscosity of 300 MPa.s.], 2 parts by weight of a Pt-based catalyst and 73 parts by weight of methyl ethyl ketone (MEK) was applied using an microgravure coater so as to have an average thickness of 1 .mu.m. And a hot-air drier was performed for 20 seconds at a temperature of 120 DEG C to form a releasing layer, thereby producing a releasing film including a releasing layer formed on the base film.

Comparative Example 2

The release film according to Example 5 was prepared in Comparative Example 1, except that the release layer was applied to have an average thickness of 1.5 탆, by performing the same process as in Comparative Example 1.

Comparative Example 3

A release film according to Example 5 was prepared in Comparative Example 1, except that the release layer was applied to have an average thickness of 2 탆, by performing the same process as in Comparative Example 1.

Comparative Example 4

After the polyester base film was subjected to corona discharge treatment, 20 parts by weight of a solvent-free silicone release agent (Shin-Etsu, KNS 1724, weight average molecular weight: 10,000 to 20,000, Viscosity of 300 MPa.s.], 2 parts by weight of a Pt-based catalyst and 78 parts by weight of methyl ethyl ketone (MEK) was applied using an microgravure coater so as to have an average thickness of 1 mu m. And a hot-air drier was performed for 20 seconds at a temperature of 120 DEG C to form a releasing layer, thereby producing a releasing film including a releasing layer formed on the base film.

Comparative Example 5

After the polyester base film was subjected to corona discharge treatment, 100 parts by weight of the polyester base film solvent-type siloxane release agent (Shin-Etsu, 3755) and 3 parts by weight of the Pt-based catalyst were mixed with toluene and methyl ethyl ketone (MEK) Was diluted in 77 parts by weight of a mixed solvent to prepare a release composition, and the release composition was applied to the polyester base film using an microgravure coater so as to have an average thickness of 1 mu m. Thereafter, the composition was dried by hot air for 20 seconds at a temperature of 120 캜 to form a release layer, thereby producing a release film comprising a release layer formed on the base film.

The difference between the release films according to Comparative Examples 1 to 5 is shown in Table 1 below.

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Type and content of release agent Dance Formulation
25 parts by weight of silicone
Dance Formulation
silicon
25 parts by weight
Dance Formulation
silicon
25 parts by weight
Dance Formulation
silicon
20 parts by weight
Solvent type
Siloxane
100 parts by weight
Silica bead content (parts by weight) - - - - - Composition average coating thickness
(μm)
One 1.5 2 1.5 One

Experimental Example

(1) Surface experiment of release film

1) Surface observation experiment according to the average coating thickness of the mold release composition

The surfaces of the release films according to Examples 2, 5 and 6 were measured by SEM and are shown in Figures 2a to 2c. Specifically, the release film according to Example 5 is shown in Fig. 2B, the release film according to Example 2 is shown in Fig. 2A, and the release film according to Example 6 is shown in Fig. 2C.

2A to 2C, the silicon ratios were visually confirmed, and it was confirmed that the silicone beads of the release film according to Example 5 (that is, the case where the release composition was coated at 1 μm) were most noticeable .

2) Surface observation experiment according to the content of silica beads in the mold release composition

The surfaces of the release films according to Examples 2 to 4 were measured by SEM and are shown in Figs. 3A to 3C. Specifically, the release film according to Example 2 is shown in Fig. 3A, the release film according to Example 3 is shown in Fig. 3B, and the release film according to Example 4 is shown in Fig. 3C.

3A to 3C, the silicon beads could be visually confirmed, and it was confirmed that the silicone beads of the release film according to Example 4 (in other words, the release composition containing 1 part by weight of silicon beads) were most noticeable I could.

 (2) Measurement of physical properties of release film

(1) releasing force, (2) residual adhesion, (3) adhesion, (4) curability and (5) blocking properties of the release films prepared according to Examples 4 to 6 and Comparative Examples 1 to 5 were measured and described in Table 3.

Each concrete measurement method is as follows.

① Release force

The releasing force (peeling force) was based on FINAT-10, and a standard tape (TESA7475-acrylic system) having a width of 50 mm and a length of 175 mm was attached to the release layer of each specimen. Then, a standard tape was pressed on the test piece by reciprocating twice at a speed of 10 mm / sec using a FINAT test roller (2 Kg load), and then a specimen was sandwiched between two flat metal plates for sufficient compression of the release layer of each specimen and the standard tape And stored at a temperature of about 23 캜 for 20 hours under a pressure of 70 g / cm 2. Thereafter, the pressure was removed, and after 4 hours, the specimen was fixed to the jig, and then the standard tape was peeled off at a rate of 300 mm / min in the direction of 180 degrees.

The average value (g / inch) of each specimen is shown in Table 3 below.

② Residual Adhesion Ratio

A standard adhesive tape (No. 31B) was affixed to the release layer of each specimen, and residual adhesive force and underlying adhesive force were measured at 22 ° C and 55% RH under constant temperature and humidity conditions as follows.

 - Residual adhesive force: No adhesion to each release layer of each specimen. The 3LB adhesive tape was cyclically pressed once with a 2 kg rubber roller, heat treated at lOO < 0 > C for 1 hour, and then the specimen was peeled from the pressed sample. The adhesive strength to the 3lB adhesive tape was measured. That is, the specimen was peeled off and the above No. The 3lB adhesive tape was pressed and attached to a metal plate, and then the adhesive strength was measured by pulling off at 180 degrees, and the measured value was regarded as the residual adhesive force.

- Adhesive strength: Adhesive tape (No. 31B) as in the case of residual adhesive strength is used. The adhesive strength is measured by a method in which the adhesive tape is pressed on a metal plate and then pulled off at 180 degrees. As an adhesive strength.

The residual adhesive force and the base adhesive force were calculated according to the following formula, and the results are shown in Table 3 below.

Residual adhesion rate (%) = (residual adhesive force / base adhesive force) X 100

③ Adhesiveness

After the curing of each release film, the surface of the release layer was rubbed strongly against the release film for 24 hours at a temperature of 60 캜 for ten times, and the fog or fall-off of the release layer surface was visually observed. And the results are shown in Table 3 below. In this case, " o " means blurring and no dropout, " blur ", and " X " means dropout.

④ Hardness

After each release film was cured, the surface of the release layer was strongly rubbed ten times, and the fog or fall-off of the release layer surface was visually observed and evaluated according to the following criteria. The results are shown in Table 3 below.

In this case, " o " means blurring and no dropout, " blur ", and " X " means dropout.

⑤ Blocking

After curing each release film, the surface of the release layer and the surface of the non-release layer were overlapped with each other for 1 to 5 times with respect to the release film that had passed for 24 hours at a temperature of 60 ° C. (Non-releasing layer) was observed and evaluated according to the following criteria. The results are shown in Table 3 below. At this time, the steel means a state in which the interface between the release layer and the non-formation type layer strongly adheres to each other, there is no air layer between the interfaces, and there is no slip property (that is, The drug means a state in which the interface between the releasing layer and the non-releasing layer strongly adheres, there is no air layer locally between the interfaces, and the slipping property is normal (that is, there is a possibility that a local property abnormality is likely to occur) , And X represents a state in which an air layer exists between the release layer and the non-aliased layer interface and the slip property is good (that is, the property is not likely to occur).

Evaluation items Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Release force
(g / inch)
3.4 2.8 3.2 3.8 3.7 4.0 4.6 4.6 5.6 - 5.4
Residual sticking rate
(%)
94 95 95 96 95 92 93 94 94 - 62
Adhesiveness × - Hardenability - blocking River none none none about about River River River - none Remarks - - - - - - - - - Local aggregation (no work) -

As shown in Table 3, it was confirmed that the release films according to Examples 1 to 6 exhibit excellent adhesion due to low releasing force. In addition, it was confirmed that the release films according to Examples 1 to 6 not only had a low residual adhesion, but also had excellent curability. In addition, it was confirmed that the release films according to Examples 1 to 6 have no or less blocking than the release films according to Comparative Examples 1 to 5. In the case of the comparative examples, it was confirmed that all the blocking occurred strongly, making it difficult to use as a product.

(3) Measurement of release force according to mold release speed

The releasing force test according to the releasing speed was performed using the releasing film produced according to Example 2 and Comparative Example 5.

Specifically, based on FINAT-10, a standard tape (TESA7475-acrylic system) having a width of 50 mm and a length of 175 mm was attached to the silicone release layer of the specimen prepared according to Example 2 and Comparative Example 5 first. Then, the standard tape was pressed onto the specimen by reciprocating twice at a speed of 10 mm / sec using a FINAT test roller (2 Kg load), and then a specimen was put between two flat metal plates for sufficient compression of the silicon release layer and the standard tape Cm < 2 > at a temperature of about 23 [deg.] C for 20 hours. After removing the pressure, the specimen was fixed to the jig 4 hours later, and then the standard tape was peeled off at a speed of 300, 3000, and 30000 mm / min in a direction of 180 degrees.

4, it was confirmed that the releasing force of the release film produced according to Example 2 is excellent regardless of the release speed. In addition, the release force of the release film produced according to Example 2 was found to be much larger than the release force of the release film prepared according to Comparative Example 5 as the release speed increased.

The embodiments of the present invention described above should not be construed as limiting the technical idea of the present invention. The scope of protection of the present invention is limited only by the matters described in the claims, and those skilled in the art will be able to modify the technical idea of the present invention in various forms. Accordingly, such improvements and modifications will fall within the scope of protection of the present invention as long as it is obvious to those skilled in the art.

10: substrate film
20: metal oxide particles
30:
100: release film

Claims (13)

A base film; And
A release film formed on the base film and comprising a release layer comprising a solventless silicone release agent and metal oxide particles,
The release layer has an average thickness of 0.07 to 2 m,
The metal oxide particles have an average particle diameter of 2 to 5 mu m,
Wherein the average particle diameter of the metal oxide particles is larger than the average thickness of the release layer,
Wherein said solventless silicone release agent has a viscosity at 25 DEG C of from 200 to 1,000 mPa.s,
Wherein the solventless silicone release agent has a weight average molecular weight of 10,000 to 20,000.
The method according to claim 1,
Wherein the metal oxide particles are metal oxide beads.
The method according to claim 1,
Wherein the base film is a corona discharge treated polyester film.
The method according to claim 1,
Wherein the solvent-free silicone release agent and the metal oxide particles are mixed in a proportion of 30 to 50: 0.1 to 2 parts by weight in the release layer, respectively.
delete delete The method according to claim 1,
Wherein the metal oxide particles comprise at least one selected from the group consisting of silica, titanium dioxide (TiO 2 ), aluminum oxide (Al 2 O 3 ), and zinc dioxide (ZnO 2 ).
The method according to claim 1,
Wherein said solventless silicone release agent is a siloxane-based release agent.
Applying a releasing composition comprising a solventless silicone release agent, metal oxide particles, a metal catalyst and a solvent on a substrate film; And
Drying the releasing composition to form a release layer; / RTI >
The release layer has a thickness of 0.07 to 2 m,
The metal oxide particles have an average particle diameter of 2 to 5 mu m,
Wherein the average particle diameter of the metal oxide particles is larger than the average thickness of the release layer,
Wherein said solventless silicone release agent has a viscosity at 25 DEG C of from 200 to 1,000 mPa.s,
Wherein the solventless silicone release agent has a weight average molecular weight of 10,000 to 20,000.
10. The method of claim 9,
The release composition comprises, in 100 parts by weight of the release composition, 30 to 50 parts by weight of a silicone release agent, 0.1 to 2 parts by weight of a metal oxide particle, 5 to 10 parts by weight of a metal catalyst, and 30 to 50 parts by weight of a solvent Way.
10. The method of claim 9,
Wherein the mold-releasing composition has a viscosity of from 50 to 100 MPa.s at 25 占 폚.
10. The method of claim 9,
Wherein the step of drying the mold-releasing composition is performed at a temperature of 110 to 130 캜.
10. The method of claim 9,
Wherein the step of applying the releasing composition is carried out through a microgravure coating process.
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KR20190041827A (en) * 2017-10-13 2019-04-23 김윤일 Releasing film with improved slippage and manufacturing method thereof
KR20190123079A (en) 2018-04-23 2019-10-31 도레이첨단소재 주식회사 Release film and manufacturing method thereof
KR20190143676A (en) * 2018-06-21 2019-12-31 도레이첨단소재 주식회사 Release film
KR20200015215A (en) * 2018-08-03 2020-02-12 (주)케이에프엠 Release film patterned and Tape comprising the same
KR20200016320A (en) 2020-02-07 2020-02-14 도레이첨단소재 주식회사 Release film and manufacturing method thereof
CN111748278A (en) * 2020-07-07 2020-10-09 浙江洁美电子科技股份有限公司 Release agent for quickly stripping OCA (optical clear adhesive) and release film containing same
KR20210120717A (en) * 2020-03-27 2021-10-07 도레이첨단소재 주식회사 Release film and manufacturing method thereof
CN113910608A (en) * 2021-10-10 2022-01-11 北京工业大学 PDMS release film with fractal geometric micro-groove oil storage structure added on surface

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JP2006205443A (en) * 2005-01-26 2006-08-10 Oji Tokushushi Kk Double-side mold release film for correction tape
JP2011173362A (en) * 2010-02-25 2011-09-08 Fujimori Kogyo Co Ltd Mold releasing film excelling in transparency
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KR20010087777A (en) 2001-04-19 2001-09-26 이정헌 Coating Compositions for proofing adhesion of stickers
JP2006205443A (en) * 2005-01-26 2006-08-10 Oji Tokushushi Kk Double-side mold release film for correction tape
JP2011173362A (en) * 2010-02-25 2011-09-08 Fujimori Kogyo Co Ltd Mold releasing film excelling in transparency
KR20140105819A (en) * 2011-12-09 2014-09-02 씨피필름즈 인코포레이티드 Modified release coatings for optically clear film

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190041827A (en) * 2017-10-13 2019-04-23 김윤일 Releasing film with improved slippage and manufacturing method thereof
KR102006776B1 (en) * 2017-10-13 2019-08-02 김윤일 Releasing film with improved slippage and manufacturing method thereof
KR20190123079A (en) 2018-04-23 2019-10-31 도레이첨단소재 주식회사 Release film and manufacturing method thereof
KR102132282B1 (en) * 2018-06-21 2020-08-05 도레이첨단소재 주식회사 Release film
KR20190143676A (en) * 2018-06-21 2019-12-31 도레이첨단소재 주식회사 Release film
KR20200015215A (en) * 2018-08-03 2020-02-12 (주)케이에프엠 Release film patterned and Tape comprising the same
KR102511351B1 (en) 2018-08-03 2023-03-17 (주)케이에프엠 Release film patterned and Tape comprising the same
KR20200016320A (en) 2020-02-07 2020-02-14 도레이첨단소재 주식회사 Release film and manufacturing method thereof
KR20210120717A (en) * 2020-03-27 2021-10-07 도레이첨단소재 주식회사 Release film and manufacturing method thereof
KR102390420B1 (en) 2020-03-27 2022-04-25 도레이첨단소재 주식회사 Release film and manufacturing method thereof
CN111748278A (en) * 2020-07-07 2020-10-09 浙江洁美电子科技股份有限公司 Release agent for quickly stripping OCA (optical clear adhesive) and release film containing same
CN113910608A (en) * 2021-10-10 2022-01-11 北京工业大学 PDMS release film with fractal geometric micro-groove oil storage structure added on surface
CN113910608B (en) * 2021-10-10 2023-09-19 北京工业大学 PDMS release film with fractal geometric micro-groove oil storage structure added on surface

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