KR101968546B1 - The method for measuring the temporal stability of release film - Google Patents

Abstract

Providing a release film comprising a substrate layer and a release layer; Preparing a laminate having an adhesive layer on one side of the release layer; Storing the first laminate at a first temperature of 20 ° C to 40 ° C for a first period of time ranging from 20 hours to 30 hours, and then measuring a first releasing force; Storing the second laminate at a second temperature higher than the first temperature by 20 ° C to 80 ° C for a second period of time that is longer by 48 hours to 144 hours than the first time and then measuring a second release force; Measuring an aging change rate according to the following formula 1; And evaluating the stability over time when the measured change rate over time is 30% or less.
[Formula 1]
% Change with time = (second releasing force - first releasing force) / first releasing force x 100

Description

TECHNICAL FIELD [0001] The present invention relates to a releasing film,

And a method for measuring the stability of the releasing film over time.

The release film facilitates the handling and transportation of the product, and can be easily separated and used for various purposes. For example, such a release film can be used as a carrier film of an adhesive film. In the case of judging whether or not such a release film is suitable for use as a carrier film, the release film can be easily separated even after a long time with the release film adhered to the adhesive film, Whether or not to give is one of the important factors. Therefore, there is a need for a method for judging whether or not it is qualified as a release film before processing into a product.

One embodiment of the present invention provides a method for measuring aging stability, which can effectively determine whether or not the release film is easily deformable without being deformed according to the passage of time before processing the product into a product.

In one embodiment of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: providing a release film comprising a substrate layer and a release layer; Preparing a laminate having an adhesive layer on one side of the release layer; Measuring a first release force after storing the first stack at a first temperature for a first time; Storing the second laminate at a second temperature higher than the first temperature for a second time longer than the first time and then measuring a second release force; Measuring an aging change rate according to the following formula 1; And evaluating the stability over time when the measured change rate over time is 30% or less.

[Formula 1]

% Change with time = (second releasing force - first releasing force) / first releasing force x 100

The difference between the first temperature and the second temperature may be from about 20 ° C to about 80 ° C, and the difference between the first and second times may be from about 48 hours to about 144 hours.

The first temperature may be from about 20 [deg.] C to about 40 [deg.] C, and the first time may be from about 20 hours to about 30 hours.

The second temperature may be from about 40 ° C to about 120 ° C, and the second time may be from about 68 hours to about 174 hours.

Wherein the releasing layer is at least one selected from the group consisting of a silicone releasing agent, a melamine releasing agent, a polyolefin releasing agent, an epoxy releasing agent, an acrylic releasing agent, a fluorine releasing agent, a cellulose releasing agent, a paraffin releasing agent, an epoxy- .

The base layer may comprise at least one selected from the group consisting of paper, nonwoven fabric, polyethylene terephthalate (PET), polyethylene (PE), polyvinyl alcohol (PVA), and combinations thereof.

The adhesive layer may include at least one selected from the group consisting of an acrylic adhesive, a silicone adhesive, a rubber adhesive, and a combination thereof.

The method for measuring the stability with time of the releasing film provides a method for determining whether the releasing film has appropriate stability over time before processing into a product, thereby reducing the defective rate of the product containing the releasing film, have.

In addition, a release film having a long-term stability measured according to the above-described measurement method satisfies specific conditions can be utilized for various applications based on excellent physical properties.

FIG. 1 schematically shows a method for measuring the stability of a release film according to an embodiment of the present invention.
2 is a cross-sectional view schematically showing an embodiment of a release film used in the method for measuring the stability of the releasing film with time.
3 is a cross-sectional view schematically showing one embodiment of the laminate used in the method for measuring the stability of the release film with time.

BRIEF DESCRIPTION OF THE DRAWINGS The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the attached drawings in which: These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art to which the invention pertains. Only. Like reference numerals refer to like elements throughout the specification.

One embodiment of the present invention provides a method of manufacturing a semiconductor device, comprising: providing a release film comprising a substrate layer and a release layer; Preparing a laminate having an adhesive layer on one side of the release layer; Measuring a first release force after storing the first stack at a first temperature for a first time; Storing the second laminate at a second temperature higher than the first temperature for a second time longer than the first time and then measuring a second release force; And measuring an aging rate by the following general formula (1).

[Formula 1]

% Change with time = (second releasing force - first releasing force) / first releasing force x 100

The release film facilitates the handling and transportation of the product, and can be easily separated, and can be used for various purposes, and is widely used as a carrier for the adhesive layer. However, when the release film is attached to the adhesive layer and transported, the functional groups remaining on the release film may react with the components of the adhesive layer over time, which may cause adhesion when the release film is peeled The aging problem may occur where the layer is damaged or is not easily separated.

On the other hand, in the method of measuring the stability with time of the release film, it is determined through a simple method whether the release film has suitable physical properties as a carrier use of the adhesive layer. The stability of the releasing film over time can be determined in advance through the above-described measuring method. From this, the defective rate of the product including the releasing film can be reduced and the reliability can be improved.

FIG. 1 schematically shows a method for measuring the stability with time of the releasing film. Referring to FIG. 1, the method of measurement may comprise providing a release film 100 comprising a substrate layer 10 and a release layer 20. The release film 100 may include the base layer 10 and the release layer 20 formed on one surface of the base layer 10 as an object of the stability over time.

The measuring method may include the step of preparing a laminate 200 having an adhesive layer 30 on one surface of a release layer 20 of the release film 100. The release film 100 may be used as a carrier of a pressure sensitive adhesive film. The pressure sensitive adhesive layer 30 may be handled and transported using the release film 100, An adhesive tape including the adhesive layer 30 may be attached to one surface of the layer 20.

FIG. 2 schematically shows an embodiment of a release film 100 used in the method of measuring stability with time of the release film. FIG. 3 is a cross-sectional view of a release film 20 of the release film, And is a schematic representation of an embodiment of the laminate 200.

Referring to Fig. 1, the above-mentioned measuring method can be referred to as a first laminate and a second laminate, respectively, by preparing two of the laminate in the same manner, and the first laminate and the second laminate are made to be different from each other Environment. ≪ / RTI >

Specifically, the first laminate is stored at a first temperature for a first time, and the second laminate is stored at a second temperature higher than the first temperature for a second time that is longer than the first time . In addition, the measurement method can measure the first releasing force and the second releasing force after storing the first laminate and the second laminate in different environments, respectively.

By storing the first laminate and the second laminate in different environments as described above, accurate and reliable results can be obtained in determining the stability over time with temperature and time.

Specifically, the first releasing force and the second releasing force are the release force between the releasing layer 20 and the pressure-sensitive adhesive layer 30 of the first laminate and the second laminate, respectively.

The aging stability measuring method may include measuring an aging change rate according to the general formula (1) using the first releasing force and the second releasing force. The aged change rate indicates the degree of change of mold releasing force according to the storage time and the temperature change, and the smaller the degree, the better the aging stability.

The first laminate and the second laminate may be stored at a first temperature and a second temperature, respectively, and the second temperature may be higher than the first temperature. Specifically, the difference between the first temperature and the second temperature may be between about 20 캜 and about 80 캜.

In addition, the first laminate and the second laminate may be stored for a first time and a second time, respectively, and the second time may be longer than the first time. Specifically, the difference between the first time and the second time may be from about 48 hours to about 144 hours .

When the difference between the first temperature and the second temperature and the difference between the first time and the second time all satisfy the above range, due to the difference in the environment in which the first laminate and the second laminate are stored The stability over time can be effectively measured and judged, and a reliable result can be obtained.

Specifically, the stability of the releasing film with respect to time may be measured by storing the first laminate at the first temperature for a first time, and the first time may be about 20 hours to about 30 hours. In general, the releasing film may start to change in releasing force after a lapse of the time in the range after application, and the first releasing force may be measured after storing the first laminate for the time in the range, A reasonable reference value of the measurement can be derived.

Also, the first temperature may be between about 20 ° C and about 40 ° C. The range of the first temperature is close to the range of room temperature and the time point at which the release force of the release film is changed can be effectively detected by keeping the first laminate at the temperature within the range for the first time, A reasonable reference value of the measurement can be derived.

The stability of the release film over time may be such that the second laminate is kept at the second temperature for a second time, and the second time may be from about 68 hours to about 174 hours. The releasing film may have a maximum change in releasing force at a time point after the application of the releasing film has elapsed after the application of the releasing film, and the second releasing force may be measured after storing the second laminate for the time period It is possible to derive a reasonable reference value.

Also, the second temperature may be between about 40 ° C and about 120 ° C. By keeping the release film in the range of the second temperature for the second time, it is possible to effectively detect the time point at which the release force is maximally changed, and it is possible to derive a reasonable reference value for the measurement of the rate of change with time.

2 schematically shows one embodiment of the release film used in the method for measuring the stability of the releasing film over time.

The release film 100 may include a base layer 10 and a release layer 20. The release layer 20 to be subjected to the release force measurement may be a silicone release agent, An epoxy-based releasing agent, an acrylic-based releasing agent, a fluorine-based releasing agent, a cellulose-based releasing agent, a paraffin-based releasing agent, an epoxy-melamine-based releasing agent and a combination thereof.

For example, the release layer 20 may include a silicone-based release agent. In this case, the stability of the release film can be measured by a method of measuring the stability with time, and a high accuracy and reliability can be obtained.

Specifically, the base layer 10 may include at least one selected from the group consisting of paper, nonwoven fabric, polyethylene terephthalate (PET), polyethylene (PE), polyvinyl alcohol (PVA), and combinations thereof.

For example, the base layer 10 may include polyethylene terephthalate (PET) or polyethylene (PE). In this case, the base layer 10 has excellent heat resistance, excellent mechanical properties and other stability, Accurate and reliable results can be obtained through measurement methods.

The releasing film 100 may be used as a carrier film of an adhesive film. In this regard, the aging stability measuring method may be a method of measuring the aging stability of a laminated body 200 including an adhesive layer 30 on one side of the releasing layer 20, . ≪ / RTI >

Specifically, the pressure-sensitive adhesive layer 30 may include at least one selected from the group consisting of an acrylic pressure-sensitive adhesive, a silicone pressure-sensitive adhesive, a rubber pressure-sensitive adhesive, and combinations thereof.

For example, the pressure-sensitive adhesive layer 30 may include an acrylic pressure-sensitive adhesive. In this case, the pressure-sensitive adhesive layer 30 may be advantageous from the viewpoint of securing the versatility of the method of measuring the stability over time, and reliable results can be obtained.

Another embodiment of the present invention can provide a release film having an elapsed time change rate of about 30% or less as measured according to the method for measuring stability with time of release film.

The rate of change with time of the release film may be about 30% or less, for example, about 20% or less. When the release film has a time-dependent change rate in the above-mentioned range, excellent stability over time can be ensured, and when the release film is applied to a product, excellent physical properties can be realized.

Hereinafter, specific embodiments of the present invention will be described. However, the embodiments described below are only intended to illustrate or explain the present invention, and thus the present invention should not be limited thereto.

Example  One

A polyethylene terephthalate (PET) base layer having a thickness of 50 mu m was provided, and a releasing film having a 200 nm thick release layer laminated with a polydimethylsiloxane (PDMS) release agent was provided on one side of the base layer. An adhesive tape (tesa7475) including an adhesive layer formed of an acrylic adhesive was prepared, and the adhesive layer was reciprocated three times with a roller of 2 kg so as to adhere to the release layer to prepare a first laminate. A second laminate having the same base layer, releasing layer and adhesive layer laminated was produced in the same manner as in the above first laminate.

After the first laminate was stored at 20 DEG C for 24 hours, the first release force between the release layer and the adhesive layer was measured. Then, after the second laminate was stored at 60 DEG C for 170 hours, the second release force between the release layer and the pressure-sensitive adhesive layer was measured.

Specifically, the first releasable force and the second releasable force were obtained by binding the adhesive layer to a jig of a measuring instrument (Chemical Instrument, AR-1000), measuring the peeling speed at 30 cm / min and the peeling angle at 180, And the force separating from the release layer was measured.

Subsequently, the aging change rate according to the general formula (1) was measured using the first releasing force and the second releasing force.

The aging rate of each of the three types of laminated samples was measured by the method of Example 1, and the composition and content of the release layer of each sample were as shown in Table 1 below.

ingredient Content [wt%] Sample 1 Sample 2 Sample 3 solvent 90 83 86 Silicon main material 9 8 9 Cross-linking agent - 8 4 catalyst One One One

Experimental Example  1: Measurement of aging stability

The first releasing force, the second releasing force and the elapsed time change rate of each sample measured in Example 1 are shown in Table 2 below. Table 2 also shows the results of judging the elapsed time stability of each sample based on the change with time. The stability with time was evaluated according to the criteria of Excellent (∘) when the change rate with time was 30% or less, △ when it was more than 30%, less than 100%, and inferiority (Х) when it was 100% or more.

Sample First release force [gf / in] Second release force [gf / in] Change over time Stability over time One 15.0 17.1 14% ○ 2 31.2 79.7 155% Χ 3 111.1 187.5 69% △

 Table 2 shows the stability of the releasing film according to the aging stability measurement method of Example 1. The stability of the releasing film with respect to time was found to be less than 30% , And the elapsed time change rate of the sample 2 was more than 100%, indicating that the stability with time was inferior. In addition, it can be seen that the elapsed time change rate of the sample 3 is in the range of more than 30% and less than 100%, so that the stability with time is normal. In this way, information on the durability according to temperature and time can be obtained in the commercialization of the release film by judging the stability with time of the sample in advance, and the defective rate of the product can be reduced. In addition, various products having excellent physical properties can be obtained by commercializing a sample having an elapsed change rate measured by the above method of not more than about 30%, for example, not more than about 20%, as a release film.

100: release film
200: laminate
10: substrate layer
20:
30: Adhesive layer

Claims (4)

Providing a release film comprising a substrate layer and a release layer;
Preparing a laminate having an adhesive layer on one side of the release layer;
Storing the first laminate at a first temperature of 20 ° C to 40 ° C for a first period of time ranging from 20 hours to 30 hours, and then measuring a first releasing force;
Storing the second laminate at a second temperature higher than the first temperature by 20 ° C to 80 ° C for a second period of time that is longer by 48 hours to 144 hours than the first time and then measuring a second release force; And
Measuring an aging rate by the following general formula 1;
And evaluating the stability over time when the measured percent change over time is 30% or less
Method for measuring stability of releasing film over time.

[Formula 1]
% Change with time = (second releasing force - first releasing force) / first releasing force x 100
The method according to claim 1,
The releasing layer includes one selected from the group consisting of a silicone-based releasing agent, a melamine-based releasing agent, a polyolefin-based releasing agent, an epoxy-based releasing agent, an acrylic releasing agent, a fluorine-based releasing agent, a cellulosic releasing agent, a paraffin-based releasing agent, an epoxy- doing
Method for measuring stability of releasing film over time.
The method according to claim 1,
Wherein the substrate layer comprises one selected from the group consisting of paper, nonwoven, polyethylene terephthalate (PET), polyethylene (PE), polyvinyl alcohol (PVA)
Method for measuring stability of releasing film over time.
The method according to claim 1,
Wherein the pressure-sensitive adhesive layer comprises one selected from the group consisting of an acrylic pressure-sensitive adhesive, a silicone pressure-sensitive adhesive, a rubber pressure-sensitive adhesive,
Method for measuring stability of releasing film over time.

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