JP2013036813A - Gas permeability test piece, producing method of gas permeability test piece, gas permeability test piece producing device, and gas permeability evaluating device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a gas permeability test piece capable of reducing an influence of gas entering from a film end surface, and further accurately evaluating gas permeability; a producing method of the gas permeability test piece; a gas permeability test piece producing device; and a gas barrier permeability evaluating device.SOLUTION: A gas permeability test piece 100 includes: a film 21; a corrosive metal layer 22 formed on at least a part of one surface 21b of the film 21; and a low gass permeable non-corrosive material 23 for sealing the corrosive metal layer 22 and the one surface 21b of the film 21 on which the corrosive metal layer 22 is formed. An end surface 21a of the film 21 is sealed by the low gas permeable non-corrosive material 23.

Description

  The present invention relates to a gas permeable test piece for evaluating gas permeability by measuring a corrosion state of a metal, a method for producing the gas permeable test piece, a gas permeable test piece creating apparatus, and a gas barrier permeability evaluating apparatus.

  A metal corrosion method typified by a calcium corrosion method is known as a gas barrier property evaluation method for a film (see, for example, Patent Document 1). This method is an evaluation method for obtaining the gas barrier property of a film by measuring the amount of the corroded metal by reacting the target gas permeated through the target film with the corrosive metal. Specifically, as shown in FIGS. 5 and 6, the corrosive metals 2 and 12 are sealed with the low gas permeable non-corrosive materials 3 and 13 so as to react only with the gas that has permeated the target films 1 and 11, respectively. Create a test specimen. Thereafter, these test pieces are exposed to a constant gas concentration and a constant temperature condition, and the target gas is permeated from the measurement surfaces of the target films 1 and 11 to corrode the corrosive metals 2 and 12, respectively. Then, the gas permeability of the target films 1 and 11 is evaluated by measuring the change over time of the corroded metal area, absorbance, electrical characteristics, and the like.

  Films having a gas barrier function are used as packaging materials for foodstuffs, precision electronic components and pharmaceuticals. In order to suppress the alteration of the contents and maintain the functions and properties of the contents, it is necessary to prevent the influence of the gas passing through the packaging material, and shut off the gas that adversely affects the functions of the contents. It has been required to have a gas barrier property. Furthermore, in recent years, films having gas barrier properties have come to be used as industrial material applications such as back surface protection sheets, which are members of solar cell modules, and gas barrier layers of organic EL elements.

In the metal corrosion method for evaluating the gas permeability of the film, as described above, it is necessary to prepare a test piece in which the corrosive metals 2 and 12 are sealed so as to react only with the gas permeated from the measurement surface of the film.
However, when the films 1 and 11 are thick, as shown in FIG. 5 and FIG. 6, the gas permeated from the film end surface reacts with the corrosive metals 2 and 12, and the gas permeability is accurately set. It had the problem that it could not be evaluated. In FIGS. 5 and 6, the paths of gas permeated from the measurement surface side of the film are shown as gas permeation paths 4 and 14, respectively. Moreover, the path | route of the gas which permeate | transmitted from the end surface side of the film is shown as the gas permeation | transmission path | routes 5 and 15, respectively.

Japanese Patent No. 4470707

  The present invention has been made to solve the above-mentioned problems, and reduces the influence of gas entering from the film end face, and more accurately evaluates gas permeability, and its gas permeability An object of the present invention is to provide a method for producing a test piece, a gas permeability test piece preparation device, and a gas barrier permeability evaluation device.

  One aspect of the present invention for solving the above problems is a film, a corrosive metal layer formed on at least a part of one surface of the film, which corrodes by reacting with a specific gas, and the corrosive property. Gas permeation for evaluating the permeability to the film, comprising a metal layer and one surface of the film on which the corrosive metal layer is formed, and a low gas permeation non-corrosive material that does not react with the gas. A gas permeable test piece, wherein an end face of the film is sealed with the low gas permeable non-corrosive material.

  According to the above aspect, the corrosive metal layer, the one surface of the film on which the corrosive metal layer is formed, and the end surface of the film are sealed with the low gas permeation non-corrosive material. For this reason, when the gas permeable test piece is exposed to a constant gas concentration and a constant temperature, it is possible to prevent gas from entering from the film end face. As a result, the gas permeates only from the measurement surface side of the film that is not covered with the low gas permeation non-corrosive material. Therefore, if it is a gas-permeable test piece which concerns on the said aspect, compared with a prior art, more exact gas-permeability can be evaluated.

  Another aspect of the present invention is a cup-shaped low gas permeation non-corrosive material that does not react with a specific gas, and an inner surface of the low gas permeation non-corrosive material. In addition, a gas permeable test piece for evaluating the transmittance of the film, comprising a corrosive metal layer that reacts with the gas and corrodes, and a film that closes the opening and seals the corrosive metal layer. A gas permeable test piece wherein the end face of the film is sealed with the low gas permeable non-corrosive material.

  According to the above aspect, the corrosive metal layer is sealed with a film, and the film end face is sealed with a low gas permeation non-corrosive material. For this reason, when the gas permeable test piece is exposed to a constant gas concentration and a constant temperature, it is possible to prevent gas from entering from the film end face. Therefore, if it is a gas-permeable test piece which concerns on the said aspect, compared with a prior art, more exact gas-permeability can be evaluated.

Here, the “cup shape” refers to a space in which the area of the cross section perpendicular to the axis from the bottom surface side to the opening side of the low gas permeation non-corrosive material is constant from the bottom surface side to the opening side. A surrounding shape or a shape surrounding a space that increases continuously or stepwise from the bottom side toward the opening side.
In another aspect of the present invention, the corrosive metal layer may include any one of an alkali metal, an alkaline earth metal, or any alloy thereof.

According to the above aspect, since the corrosive metal layer includes any one of alkali metal, alkaline earth metal, or any alloy thereof, the corrosive metal layer is corroded by water vapor. For this reason, if it is a gas-permeable test piece which concerns on the said aspect, compared with a prior art, water vapor permeability can be calculated | required easily.
In another aspect of the present invention, the alkaline earth metal may include any one of calcium, magnesium, or any alloy thereof.

  According to the above aspect, since the alkaline earth metal includes any one of calcium, magnesium, or any alloy thereof, the corrosive metal layer is corroded by water vapor. Further, the corrosive metal layer can be manufactured at a low cost. For this reason, if it is a gas-permeable test piece which concerns on the said aspect, compared with the prior art, water vapor permeability can be calculated | required cheaply and easily.

According to another aspect of the present invention, in the method for producing a gas permeable test piece according to the above aspect, the low gas permeable non-corrosive material for sealing the end face of the film is formed by chemical vapor deposition (CVD), plasma chemistry. Vapor Deposition (PECVD), Low Pressure Chemical Vapor Deposition (LPCVD), Low Pressure Chemical Vapor Deposition (SACVD), UV Assisted Chemical Vapor Deposition, Filament Assisted Chemical Vapor Deposition (FACVD), Atmospheric Pressure Chemical Vapor Deposition (APCVD) ), Atomic layer deposition (ALD), and plasma atomic layer deposition (PEALD).

According to the said aspect, since the said method is a method excellent in level | step difference covering property, a film end surface can be covered using a low gas-permeable non-corrosive material. For this reason, if it is the preparation method of the gas-permeable test piece which concerns on the said aspect, the gas-permeable test piece by which the film end surface was sealed with the low gas-permeable non-corrosive material can be produced.
Another aspect of the present invention provides a gas permeable test piece creating apparatus for producing the gas permeable test piece of the above aspect, a container in which the film is stored, and the film disposed in the container. An apparatus for forming the corrosive metal layer on one surface side, and an apparatus for forming the low gas permeation non-corrosive material disposed in the container so as to seal an end surface of the film. This is a gas permeable test piece preparation device.

According to the said aspect, a film end surface can be sealed using a low gas permeable non-corrosive material. For this reason, if it is a gas-permeable test piece preparation apparatus which concerns on the said aspect, the gas-permeable test piece which can evaluate gas permeability more correctly can be produced.
Here, “to form the corrosive metal layer on one surface side of the film” means that the corrosive metal layer may be formed in contact with one surface of the film, A gap may be formed between the corrosive metal layer.

  Further, another aspect of the present invention is that the gas permeable test piece preparation apparatus of the above aspect and the gas permeable test piece prepared by the gas permeable test piece preparation apparatus are combined with the gas permeable test piece preparation apparatus. A device that is exposed to an environment having a constant gas concentration and a constant temperature while being stored in the container, and a measuring device that measures the degree of corrosion of the corrosive metal layer in the exposed state. It is a gas permeability evaluation apparatus characterized by comprising.

  According to the above aspect, corrosion proceeds by using an apparatus that can directly expose a gas permeable test piece prepared by a gas permeable test piece preparation apparatus to an environment having a constant gas concentration and a constant temperature. The gas permeability can be evaluated by measuring the degree to which it is performed over time. For this reason, with the gas permeability evaluation apparatus according to the above aspect, it is possible to suppress the influence on the gas permeability of the environmental change due to the gas permeability test piece being exposed to the outside of the environment, and more accurate evaluation. It can be performed.

  By using the gas permeable test piece according to the present invention, gas can be prevented from permeating from the film end face, and more accurate gas permeability can be evaluated.

1 is a cross-sectional view of a gas permeability test piece according to a first embodiment. It is sectional drawing of the gas-permeable test piece which concerns on 2nd Embodiment. It is sectional drawing of the preparation apparatus of the gas-permeable test piece which concerns on 1st, 2nd embodiment. It is sectional drawing of the preparation apparatus of the gas-permeable test piece which concerns on 1st, 2nd embodiment. It is sectional drawing of the gas-permeable test piece used for the existing metal corrosion method. It is sectional drawing of the gas-permeable test piece used for the existing metal corrosion method.

Hereinafter, embodiments of the present invention will be described, but the present invention is not limited by the following embodiments, and is appropriately selected according to the type and use of the film.
<First Embodiment>
(Gas permeability test piece)
FIG. 1 is a cross-sectional view of a gas permeable test piece 100 according to the first embodiment of the present invention. As shown in FIG. 1, the gas permeable test piece 100 includes a film 21, a corrosive metal layer 22, and a low gas permeable non-corrosive material 23.
A planar corrosive metal layer 22 is provided in contact with the surface 21b on at least a part of one surface 21b of the film 21 to be measured. The low gas permeation non-corrosive material 23 is provided so as to cover the corrosive metal layer 22 and a portion of the one surface 21b of the film 21 where the corrosive metal layer 22 is not provided. Further, the end face 21a of the film is covered with a low gas permeation non-corrosive material 23 as shown in FIG.

  In other words, the gas permeable test piece 100 shown in FIG. 1 has a corrosive metal layer 22 that reacts with a specific gas and corrodes on one surface 21 b of the film 21. Furthermore, the low gas permeation which does not react with a specific gas so as to cover the corrosive metal layer 22 and the film 21 excluding the surface 21c opposite to the surface 21b in contact with the corrosive metal layer 22 (that is, the measurement surface) 21c. By forming the non-corrosive material 23, the corrosive metal 22 is sealed with the film 21 and the low gas permeation non-corrosive material 23.

  As described above, according to the above embodiment, the corrosive metal layer 22, the one surface 21 b of the film 21 on which the corrosive metal layer 22 is formed, and the end surface 21 a of the film 22 are connected to the low gas permeable non-corrosive material 23. Can be sealed with. For this reason, even when the gas permeable test piece 100 is exposed to a constant gas concentration and a constant temperature, gas intrusion from the end face 21a of the film 21 can be prevented. As a result, the gas permeates only from the measurement surface 21 c side of the film 21 that is not covered with the low gas permeation non-corrosive material 23. Thus, the corrosive metal layer 22 can only react with the gas that has permeated through the film 21, as shown by path 24. Therefore, if it is the gas-permeable test piece 100 which concerns on the said embodiment, compared with a prior art, more exact gas-permeability can be evaluated.

  The corrosive metal layer 22 may be a metal layer that reacts with a specific gas and corrodes, and includes, for example, any one of an alkali metal, an alkaline earth metal, or any alloy thereof. Alkali metal, alkaline earth metal or any alloy thereof is highly reactive and easily corroded by water vapor, so it is a suitable combination for determining water vapor permeability indicating the gas permeability of water vapor. .

  Further, as the alkaline earth metal, for example, any one of calcium, magnesium and any one of alloys thereof may be used. Calcium, magnesium or any of their alloys are easily corroded by water vapor, are inexpensive, and are easy to form a thin film by vapor deposition. is there.

The low gas permeation non-corrosive material 23 may be any material that does not react with the specific gas, such as metal, metal oxide, metal nitride, and glass. The low gas permeable non-corrosive material 23 is desirably a material having as low a gas permeability as possible, but is not limited thereto.
In the above embodiment, the case where the corrosive metal layer 22 is formed on a part of the one surface 21b of the film 21 has been described, but the present invention is not limited to this. For example, the corrosive metal layer 22 may be formed on the entire one surface 21 b of the film 21.

(Gas permeability test piece creation device)
FIG. 3 is a cross-sectional view of an apparatus 300 for producing the gas permeable test piece 100 shown in FIG. The apparatus 300 forms a pedestal 51 on which a film 21 to be measured can be set, a mask 52 (hereinafter simply referred to as “mask 52”) provided with an exchange device, and a corrosive metal layer 22. An apparatus 53 (hereinafter also simply referred to as “film forming apparatus 53”), an apparatus 54 (hereinafter also simply referred to as “film forming apparatus 54”) that forms the low gas permeable non-corrosive material 23, and a temperature. The chamber 58 includes a humidity adjusting device 56 and a corrosion degree measuring device 57 inside, and a glove box 55 capable of operating the inside of the chamber 58.

The film forming apparatus 53 is arranged so that the corrosive metal layer 22 can be formed on the one surface 21 b side of the film 21 set on the pedestal 51.
The film forming device 54 is arranged so that the end surface 21 a of the film 21 can be sealed with the low gas permeable non-corrosive material 23.
The mask 52 is disposed between the pedestal 51 and the film forming apparatus 53 or the film forming apparatus 54, and is disposed so as to face the film 21 set on the pedestal 51.

The temperature / humidity adjusting device 56 is arranged so as to adjust the temperature / humidity environment inside the chamber 58.
Further, the corrosion degree measuring device 57 is arranged so that, for example, the corrosion degree of the corrosive metal layer 22 can be measured from the measurement surface side.
In other words, the gas permeable test piece 100 producing apparatus 300 is an apparatus for producing the gas permeable test piece 100 (that is, a pedestal 51, a mask 52, a film forming apparatus 53, a film forming apparatus 54, and a glove box). 55), a device for exposing the gas permeable test piece 100 to a target temperature and humidity environment (that is, the temperature / humidity adjusting device 56), and a film provided in the gas permeable test piece 100. This is a device that also has a device for measuring the corrosion degree of the corrosive metal layer 22 corroded by the permeated gas (that is, the corrosion degree measuring device 57). As described above, the creation apparatus 300 according to the present embodiment is an apparatus that can perform from the creation of the gas permeable test piece 100 to the measurement of gas permeability with one apparatus.

The “container” in the present application refers to the chamber 58, the “apparatus for forming a corrosive metal layer” refers to the film forming apparatus 53, and the “apparatus for forming a low gas permeation non-corrosive material”. Is the film forming apparatus 54.
In addition, the “apparatus exposed to an environment having a constant gas concentration and a constant temperature” in the present application refers to the temperature / humidity adjusting device 56, and “the extent to which the corrosive metal layer is corroded in the exposed state”. The “measuring device for measuring” refers to the corrosion degree measuring device 57.

As described above, according to the above-described embodiment, the film end face 21a can be sealed with the low gas permeation non-corrosive material 23. Therefore, the gas permeability test piece 100 that can evaluate the gas permeability more accurately. Can be created.
Moreover, according to the said embodiment, by using the temperature / humidity adjustment apparatus 56, the gas permeability can be evaluated by measuring the degree of corrosion over time. Furthermore, since the influence of the environmental change on the gas permeability due to the gas permeability test piece 100 being exposed outside the environment can be suppressed, more accurate evaluation can be performed.
Examples of the corrosion degree measuring device 57 include a camera for obtaining the corroded area of the corrosive metal layer 22, an absorptiometer for obtaining the absorbance of the corrosive metal layer 22, and an electrical property measuring device for the corrosive metal layer 22. However, it is not limited to these.

In addition, in order to obtain the degree of corrosion indicating the degree of progress of corrosion, there are methods for measuring the area of the corroded surface, the absorbance, and the electrical resistance, but the present invention is not limited thereto.
Moreover, although this embodiment demonstrated the preparation apparatus 300 which can perform from the preparation of the gas-permeable test piece 100 to the measurement of gas permeability, this invention is not limited to this. For example, the creation device 400 shown in FIG. 4 may be used as the creation device for the gas permeable test piece 100. The creation device 400 is a device obtained by removing the temperature / humidity adjustment device 56 and the corrosion degree measurement device 57 from the creation device 300 described above. Specifically, a pedestal 41 on which a film 21 to be measured can be set, a mask 42 provided with an exchange device, a device 43 for forming a corrosive metal layer 22, and a low gas permeation non-corrosive material 23 is a creation apparatus configured to include a chamber 48 having a device 44 for forming a film 23 therein and a glove box 45 capable of operating the inside of the chamber 48.

Further, the pedestal 41, the mask 42, the apparatus 43 for forming the corrosive metal layer 22, the apparatus 44 for forming the low gas permeable non-corrosive material 23, and the glove box 45 are the pedestal 51, mask described in the creation apparatus 300. 52, a device 53 for forming the corrosive metal layer 22, a device 54 for forming the low gas permeation non-corrosive material 23, and the glove box 55 are arranged at substantially the same positions.
As described above, even when the creation apparatus 400 is used, the gas permeable test piece 100 can be created as in the case of the creation apparatus 300.

(How to make a gas permeable specimen)
Hereinafter, a method for producing the gas permeable test piece 100 using the production apparatus 300 shown in FIG. 3 will be described.
First, the film 21 shown in FIG. 1 is set on the pedestal 51, and the mask is set so as to open at least a part of one surface 21b of the film 21 using the mask 52 provided with an exchange device.
Thereafter, the corrosive metal layer 22 is formed only on the one surface 21 b of the film 21 where the mask 52 is opened, using the apparatus 53 for forming the corrosive metal layer 22.

After film formation, the mask 52 is changed to a mask 52 that is wider than the film 21 by using an exchange device provided in the mask 52.
After that, the low gas permeable non-corrosive material is formed so as to cover the one surface 21b and the end surface 21a of the film 21 on which the corrosive metal layer 22 is formed using the apparatus 54 for forming the low gas permeable non-corrosive material 23. 23 is deposited. When forming the low gas permeable non-corrosive material 23, for example, chemical vapor deposition (CVD), plasma enhanced chemical vapor deposition (PECVD), low pressure chemical vapor deposition (LPCVD), and low pressure chemical vapor deposition (SACVD). Selected from the group consisting of UV assisted chemical vapor deposition, filament assisted chemical vapor deposition (FACVD), atmospheric pressure chemical vapor deposition (APCVD), atomic layer deposition (ALD), and plasma atomic layer deposition (PEALD) Can be used. Since the above method is excellent in step coverage, the film end surface 21a can be easily covered with a low gas permeation non-corrosive material.
As described above, according to the above embodiment, the gas permeable test piece 100 shown in FIG. 1 can be produced.

(Measurement method of corrosion degree)
After producing the gas permeable test piece 100, the temperature and humidity control device 56 shown in FIG. 3 is used to maintain the inside of the chamber 58 at a target temperature and humidity environment, and the gas permeable test piece 100 is exposed to the environment. . After exposure for a certain time, the corrosion degree of the corrosive metal layer 22 is obtained using the corrosion degree measuring device 57.

In order to obtain the degree of corrosion of the corrosive metal layer 22, various methods such as a method of comparing the area of the corroded surface, the absorbance, the electric resistance and the change with time thereof can be used. In the evaluation analysis of the present invention, as an example, the corroded metal layer 22 is image-processed to determine the corroded area. Under the present circumstances, according to patent document 1, the gas permeability T of a film is shown by (Formula 1).
T = m × (M [Gas] / M [Metal]) × (δhαρ / A) × 1 / t (Formula 1)
In the above equation, m is the valence of the corrosive metal, M [Gas] is the molecular weight of the permeate gas, and M [Me
tal] is the molecular weight of the corrosive metal, δ is the area of the corroded portion of the corrosive metal, h is the thickness of the corrosive metal, α is the thickness correction factor, ρ is the density after corrosion of the corrosive metal, and A is the corrosive metal The sum of the areas of the corroded and non-corroded parts, t represents the exposure time.
A more accurate gas permeability can be obtained by measuring the gas permeability calculated from the above corrosion area with respect to the gas permeable test piece 100 over time and taking an average. However, the present invention is not limited to the above method.

Second Embodiment
(Gas permeability test piece)
FIG. 2 is a cross-sectional view of a gas permeable test piece 200 according to the second embodiment of the present invention. As shown in FIG. 2, the corrosive metal layer 32 is formed on at least a part of the inner surface of the cup-shaped low gas permeation non-corrosive material 33 having an opening. The corrosive metal layer 32 is sealed so as to close the opening of the low gas permeable non-corrosive material 33 with the film 31. That is, the low gas permeation non-corrosive material 33 is disposed on the corrosive metal layer 32 so as to create a space between the film 31 to be measured. Further, the end face 31a of the film is covered with a low gas permeation non-corrosive material 33 as shown in FIG. For this reason, the corrosive metal layer 32 can only react with the gas that has permeated the film 31, as shown by the path 34.

  In other words, the gas permeable test piece 200 shown in FIG. 2 is made of a low gas permeable non-corrosive material 33 that does not react with a specific gas and is corroded by reacting with the gas on at least a part of the inner surface of the cup having an opening. The corrosive metal 32 is formed, and the opening is closed so that the end face of the film 31 and the cup are in contact with each other, thereby sealing the corrosive metal 32 inside the cup.

  As described above, according to the above embodiment, the opening portion of the low gas permeation non-corrosive material 33 is closed with the film 31 to seal the corrosive metal layer 32, and the end surface 31a of the film 31 is covered with the low gas permeation non-corrosion. It can be sealed with a conductive material 33. For this reason, even when the gas permeable test piece 200 is exposed to a constant gas concentration and a constant temperature, gas can be prevented from entering from the end face 31a of the film 31. Therefore, the corrosive metal layer 32 can only react with the gas that has permeated the film 31 as indicated by the path 34. Therefore, if it is the gas-permeable test piece 200 which concerns on the said embodiment, compared with a prior art, more accurate gas-permeability can be evaluated.

The film 31, the corrosive metal layer 32, and the low gas permeation non-corrosive material 33 are the same materials as the film 21, the corrosive metal layer 22, and the low gas permeation non-corrosive material 23 described in the first embodiment. Each can be used.
In the present embodiment, the shape of the low gas permeable non-corrosive material 33 is expressed as “cup shape” or “cup”. The ratio with the height of the surrounding edge is not particularly limited. For this reason, even what has what is called a "dish shape" with a low edge is contained in said "cup shape".

  Moreover, although the said embodiment demonstrated the case where the corrosive metal layer 32 was formed in a part of inner surface of the low gas permeable non-corrosive material 33, this invention is not limited to this. For example, the corrosive metal layer 32 may be formed so as to cover the entire inner surface of the low gas permeable non-corrosive material 33.

(Gas permeability test piece creation device)
The creation apparatus of the gas permeable test piece 200 is substantially the same as the creation apparatuses 300 and 400 described in the first embodiment. Therefore, the description is omitted here.
(How to make a gas permeable specimen)
Hereinafter, a method for producing the gas permeable test piece 200 using the production apparatus 300 shown in FIG. 3 will be described.
First, the opening of the cup-shaped low gas permeation non-corrosive material 33 is opposed to a device 53 for depositing the corrosive metal layer 32 (hereinafter also simply referred to as “film deposition device 53”). The low gas permeable non-corrosive material 33 is set on the base 51.
Then, using the mask 52 provided with an exchange device, the mask is set so as to open a part of the inner surface of the low gas permeation non-corrosive material 33.

Then, using the film forming apparatus 53, the corrosive metal 32 is formed only on the inner surface of the low gas permeable non-corrosive material 33 where the mask 52 is open.
After the film formation, the glove box 55 is used to bond the openings of the low gas permeable non-corrosive material 33 so as to be closed with the film 31 shown in FIG. Thereby, the corrosive metal 32 is sealed by the low gas permeation non-corrosive material 33 and the film 31.

Thereafter, the glove box 55 is used to set the low gas permeation non-corrosive material 33 and the film 31 on the pedestal 51 again. At this time, the bottom of the cup-shaped low gas permeable non-corrosive material 33 is opposed to a device 54 (hereinafter also simply referred to as “film forming device 54”) for forming the low gas permeable non-corrosive material. set.
In other words, the low gas permeation non-corrosive material 33 is set again on the pedestal 51 so that the position of the opening is opposite to the case where the corrosive metal layer 32 is formed.

And it changes to the mask 52 opened wider than the film 31 using the exchange apparatus with which the mask 52 is equipped.
Thereafter, the low gas permeable non-corrosive material 33 is deposited using the film forming apparatus 54 so as to cover the low gas permeable non-corrosive material 33 and the end face 31 a of the film 31. The low gas permeation non-corrosive material to be formed here does not have to be the same material as the cup-shaped low gas permeation non-corrosive material on which the film 31 is already pasted, for example, the measurement gas has low permeability. , Metal, metal oxide, metal nitride, glass and the like.

As described above, according to the above embodiment, the gas permeable test piece 200 shown in FIG. 2 can be produced.
When forming a low gas permeation non-corrosive material using the film forming apparatus 54, for example, as in the case of the first embodiment, for example, chemical vapor deposition (CVD), plasma chemical vapor deposition (PECVD), Low pressure chemical vapor deposition (LPCVD), low pressure chemical vapor deposition (SACVD), UV assisted chemical vapor deposition, filament assisted chemical vapor deposition (FACVD), atmospheric pressure chemical vapor deposition (APCVD), atomic layer deposition (ALD) And a method selected from the group consisting of plasma atomic layer deposition (PEALD).

(Measurement method of corrosion degree)
The measuring method of the corrosion degree of the gas permeable test piece 200 is substantially the same as the measuring method described in the first embodiment. Therefore, the description is omitted.

  The gas permeability evaluation method of the present invention can be used as a more accurate evaluation method than existing methods.

DESCRIPTION OF SYMBOLS 1 ... Film 2 ... Corrosive metal layer 3 ... Low gas permeation non-corrosive material 4 ... Gas permeation path 5 from measurement surface ... Gas permeation path 11 from end surface ... Film DESCRIPTION OF SYMBOLS 12 ... Corrosive metal layer 13 ... Low gas permeation non-corrosive material 14 ... Gas permeation path 15 from measurement surface ... Gas permeation path 21 from end surface ... Film 21a ... Film End surface 21b of the film: one surface 21c of the film ... the other surface 22 of the film ... corrosive metal layer 23 ... low gas permeation non-corrosive material 24 ... gas permeation path from the measurement surface 25 ... Gas permeation path 31 from the end face ... Film 31a ... End face 32 of the film ... Corrosive metal layer 33 ... Low gas permeation non-corrosive material 34 ... Gas from the measurement face Transmission path 41 ... Base 42 ... Mask changer 43 A device 44 for forming a corrosive metal layer ... A device 45 for forming a low gas permeation non-corrosive material 45 ... A glove box 48 ... A chamber 51 ... A pedestal 52 ... A mask changer 53 ... Equipment 54 for forming a corrosive metal layer ... Equipment 55 for forming a low gas permeation non-corrosive material ... Glove box 56 ... Temperature / humidity adjusting device 57 ... Corrosion degree measuring device 58 ... Chamber 100 ... Gas permeability test piece 200 ... Gas permeability test piece 300 ... Gas permeability test piece creation device 400 ... Gas permeability test piece creation device

Claims (7)

With film,
A corrosive metal layer formed on at least a part of one side of the film and corroding by reacting with a specific gas;
Evaluating the transmittance of the film, comprising the corrosive metal layer and a low gas permeable non-corrosive material that does not react with the gas and seals one surface of the film on which the corrosive metal layer is formed. In the gas permeable test piece to
A gas permeable test piece, wherein an end face of the film is sealed with the low gas permeable non-corrosive material. A low gas permeation non-corrosive material that does not react with a specific gas in the shape of a cup with an opening;
A corrosive metal layer formed on at least a part of the inner surface of the low gas permeation non-corrosive material and corroding by reacting with the gas;
A gas permeable test piece for evaluating the transmittance of the film, comprising a film that closes the opening and seals the corrosive metal layer.
A gas permeable test piece, wherein an end face of the film is sealed with the low gas permeable non-corrosive material.   The gas permeable test piece according to claim 1 or 2, wherein the corrosive metal layer includes any one of an alkali metal, an alkaline earth metal, or any alloy thereof.   The gas permeable test piece according to claim 3, wherein the alkaline earth metal includes any one of calcium, magnesium, or any alloy thereof. In the preparation method of the gas permeability test piece according to any one of claims 1 to 4,
The low gas permeation non-corrosive material that seals the end face of the film is formed by chemical vapor deposition (CVD), plasma enhanced chemical vapor deposition (PECVD), low pressure chemical vapor deposition (LPCVD), or reduced pressure chemical vapor deposition (SACVD). ), UV assisted chemical vapor deposition, filament assisted chemical vapor deposition (FACVD), atmospheric pressure chemical vapor deposition (APCVD), atomic layer deposition (ALD), and plasma atomic layer deposition (PEALD). A method for producing a gas permeable test piece, comprising a step of forming by a method. In the gas permeable test piece preparation apparatus which produces the gas permeable test piece as described in any one of Claims 1-4,
A container in which the film is stored;
An apparatus for forming the corrosive metal layer on one side of the film, disposed in the container;
A gas permeable test piece producing apparatus, comprising: an apparatus for forming the low gas permeable non-corrosive material so as to seal an end face of the film disposed in the container. A gas permeable test piece preparation device according to claim 6;
In a state where the gas permeable test piece prepared by the gas permeable test piece preparation apparatus is stored in the container provided in the gas permeable test piece preparation apparatus, in an environment having a constant gas concentration and a constant temperature. Equipment exposed to,
A gas permeability evaluation apparatus comprising: a measuring device that measures a degree of corrosion of the corrosive metal layer in an exposed state.

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