JP6489466B2 - Article for measuring gas permeability, gas permeation cell, gas permeability measuring apparatus and gas permeability measuring method - Google Patents

Description

  The present invention relates to an article for measuring gas permeability, a gas permeable cell, a gas permeability measuring apparatus, and a gas permeability measuring method.

  One important characteristic of a thin film material used for packaging foods, drugs, etc. is the gas permeability of water vapor, oxygen, etc. from the inside to the outside of the space surrounded by the thin film material. In recent years, thin film materials have been applied to organic EL devices, solar cells, and the like, and such precision machines particularly require thin film materials with lower gas permeability. Thus, the required gas permeability differs depending on the field to which it is applied. Therefore, in order to provide a thin film material that satisfies the gas permeability required depending on the application, it is necessary to accurately and quickly measure the gas permeability of the thin film material.

  The gas permeability of the thin film material is usually determined by exposing one surface of the thin film material to the gas to be measured (target gas) in a sealed space and detecting the target gas detected on the other surface side. It is measured by measuring the amount (for example, Patent Document 1).

  A simple example of gas permeability measurement of a thin film material will be described with reference to FIG. The measurement is performed using a gas permeable cell 120 including a chamber (supply side chamber) 101 to which the target gas is supplied and a chamber (permeation side chamber) 102 to which the permeated target gas reaches. First, the thin film material 150 to be measured is sandwiched between the supply side chamber 101 and the transmission side chamber 102 ((b) of FIG. 1). At this time, the target gas contained in the air enters the supply side chamber 101 and the permeation side chamber 102. In order to perform accurate measurement, it is necessary to remove the target gas from the supply side chamber 101 and the permeation side chamber 102 before the measurement. For example, a gas that does not include the target gas is supplied from the supply port 103 of the supply side chamber 101 and is discharged from the discharge port 104 of the supply side chamber 101 and the discharge port 105 of the transmission side chamber 102. After the target gas is sufficiently removed from the supply side chamber 101 and the permeation side chamber 102, measurement of gas permeability is started.

Japanese Patent Laying-Open No. 2005-233934 (published on September 2, 2005)

  However, when gas permeability is measured for a plurality of thin film materials 150, outside air enters the supply side chamber 101 and the permeation side chamber 102 when the thin film material 150 is replaced ((a) in FIG. 1). Therefore, every time the thin film material 150 is replaced, it is necessary to perform the above-described removal operation from scratch. When a gas that does not include the target gas is supplied from the supply port 103 of the supply side chamber 101, only the gas that has permeated the thin film material 150 flows into the permeation side chamber 102. Therefore, the gas permeability of the thin film material 150 is low. The more it takes, the longer the removal operation takes.

  The present invention has been made in view of these problems, and an object of the present invention is to provide a gas capable of shortening the time for removing the gas to be measured from the gas permeable cell before measuring the gas permeability of the thin film material. An object of the present invention is to provide an article for measuring permeability, a gas permeable cell, a gas permeability measuring device, a gas permeability measuring method, and the like.

  In order to solve the above problems, an article for measuring gas permeability according to the present invention is an article used for measuring gas permeability of a thin film material, and is fixed to an inner wall so as to cover at least a part of a space. A gas permeable first support is provided, a permeate side chamber into which the gas that has permeated the thin film material flows, and a gas permeable second gas having a gas permeability lower than that of the first support. A support.

  In the gas permeability measurement article according to the present invention, the permeation side chamber has a portion having a first inner periphery and a portion having a second inner periphery larger than the first inner periphery. The first support is fixed to a stepped portion caused by a difference between the first inner periphery and the second inner periphery, and an inner wall of a portion having the second inner periphery. preferable.

  In the gas permeability measurement article according to the present invention, it is preferable that the permeation side chamber has a holding portion for holding the second support.

  In the gas permeability measurement article according to the present invention, the second support preferably has a gas permeability of ½ or less of the first support.

In the gas permeability measuring article according to the present invention, the first support has a water vapor permeability of 2 × 10 ⁻¹⁵ mol / (m ² · s · Pa) or more and 1 × 10 ⁻⁹ mol / ( m ² · s · Pa) or less, and the second support has a water vapor permeability of 1 × 10 ⁻¹⁵ mol / (m ² · s · Pa) to 1 × 10 ⁻¹⁰ mol / (m ² · s · Pa) or less.

  In the gas permeability measurement article according to the present invention, the first support preferably has a glass transition point of 100 ° C. or higher.

  In the gas permeability measurement article according to the present invention, it is preferable that the permeation side chamber has a holding portion for holding the thin film material.

  The gas permeability measuring article according to the present invention preferably further includes a gas permeable buffer provided detachably between the thin film material and the second support.

  In the gas permeability measurement article according to the present invention, it is preferable that the permeation side chamber has a holding portion for holding the buffer body.

  In the article for measuring gas permeability according to the present invention, the buffer preferably has a durometer hardness (type A) of 90 to 20.

  In the gas permeability measurement article according to the present invention, it is preferable that the buffer has a gas permeability higher than that of the first support.

  In the gas permeability measurement article according to the present invention, the second support preferably has a durometer hardness (type A) of 90 to 20.

  The gas permeation cell according to the present invention is a gas permeation cell used for measuring the gas permeation rate of a thin film material, and is a supply in which any of the gas permeation measurement articles described above and a gas to be measured are supplied from the outside. Side chamber.

  A gas permeability measuring apparatus according to the present invention includes the above-described gas permeation cell and detection means for detecting the gas to be measured that has passed through the thin film material from the supply side chamber and reached the permeation side chamber. .

  The gas permeability measuring method according to the present invention includes a step of setting a thin film material at a predetermined position of the gas permeability measuring apparatus described above and supplying a gas to be measured to the supply side chamber.

  The gas permeability measurement method according to the present invention may further include a step of replacing the thin film material and the second support while the first support is fixed to the inner wall of the permeation side chamber. .

  According to the present invention, it is possible to shorten the time for removing the measurement target gas from the gas permeable cell before measuring the gas permeability of the thin film material.

It is the schematic which shows the structure of the gas permeability measuring apparatus which concerns on Embodiment 1 of this invention. It is the schematic which shows the structure of the gas permeable cell which concerns on Embodiment 1 of this invention. It is the schematic which shows the structure of the gas permeable cell which concerns on Embodiment 2 of this invention. It is the schematic which shows the structure of the gas permeable cell which concerns on Embodiment 3 of this invention. It is the schematic which shows the structure of the gas permeable cell which concerns on other embodiment of this invention. It is the schematic which shows the structure of the gas permeable cell which concerns on other embodiment of this invention. It is the schematic which shows the structure of the conventional gas permeability measuring apparatus.

[Gas permeability measuring device]
<Embodiment 1>
Embodiment 1 of the present invention will be described below with reference to FIGS. 1 and 2. FIG. 1 is a schematic diagram showing a configuration of a gas permeability measuring device 30 according to Embodiment 1 of the present invention. FIG. 1 is a longitudinal front view of a state in which the constituent members are assembled and a thin film material 50 to be measured is set. The gas permeability measuring device 30 includes a gas permeable cell 20 and a detector (detecting means) 21. FIG. 2 is a schematic view showing the configuration of the gas permeable cell according to Embodiment 1 of the present invention. The gas permeability measuring device 30 is a device used for measuring the gas permeability of the thin film material 50. The thin film material 50 is not included in the configuration of the gas permeability measuring device 30.

  As will be described later, the gas permeability measuring device 30 is characterized by including a permeation side chamber 2 in which a first support 3 is provided and a second support 4.

(Gas permeable cell 20)
The gas permeation cell 20 includes a supply side chamber 1, a permeation side chamber 2, a second support (second support) 4, and a buffer 5. A supply port 14 is provided in the supply side chamber 1. The transmission side chamber 2 is provided with a discharge port 15 and a first support (first support) 3. The gas permeation cell 20 is used by sandwiching a thin film material 50 to be measured for gas permeability between the supply side chamber 1 and the permeation side chamber 2. The supply side chamber 1 and the transmission side chamber 2 are provided at positions facing each other with the thin film material 50 interposed therebetween.

  The supply side chamber 1 is provided with a supply port 14 for supplying gas from the outside. In the first embodiment, as shown in FIG. 1, gas is supplied from the outside in the direction of the arrow from a supply port 14 provided on the upper surface of the supply side chamber 1, and the space 7 of the supply side chamber 1 is filled with gas. Is done. When the gas permeability of the thin film material 50 is measured, the gas to be measured is filled into the supply side chamber 1 from the outside. The gas to be measured is not particularly limited, and various gases can be filled into the supply-side chamber 1 as a measurement target. For example, water vapor, oxygen, nitrogen, helium, hydrogen, argon, carbon dioxide, Carbon monoxide and inorganic gases such as hydrogen sulfide, hydrocarbons such as methane and butane, alcohols such as ethanol, organic acids such as formic acid and acetic acid, and aromatic hydrocarbons such as benzene and toluene It is possible to suitably use a gas such as an organic gas. The outer periphery of the supply side chamber 1 is the same as or smaller than the inner periphery of the transmission side chamber 2.

  The transmission side chamber 2 is provided with a discharge port 15 for discharging gas. The discharge port 15 is connected to the detector 21 of the gas permeability measuring device 30. The gas discharged from the discharge port 15 is detected by the detector 21. In the first embodiment, as shown in FIG. 1, the gas that has passed through the thin film material 50 flows into the space 6 of the transmission side chamber 2 from the direction of the arrow, and this gas is discharged from the discharge port 15 in the direction of the arrow. The The permeation side chamber 2 is provided with a first support 3. The first support 3 is provided so as to cover the space 6 of the transmission side chamber 2.

  As shown in FIG. 2A, the permeation side chamber 2 includes three portions having different inner peripheries, that is, a portion 8 having a first inner periphery, and a second larger than the first inner periphery. A portion 9 having an inner periphery and a portion 10 having a third inner periphery larger than the second inner periphery are included. Therefore, the inner wall of the permeation side chamber 2 has a step portion 11 caused by the difference between the first inner circumference and the second inner circumference, and a step caused by the difference between the second inner circumference and the third inner circumference. It has a portion 12. The portion 10 having the third inner periphery forms a holding portion 13 for holding the second support body 4, the buffer body 5, and the thin film material 50.

  Due to the stepped portion 11, it is possible to avoid the first support 3 from being detached from the transmission side chamber 2 due to the force applied when the thin film material 50 is sandwiched between the supply side chamber 1 and the transmission side chamber 2. Due to the stepped portion 12, it is possible to reduce the outside air from leaking into the space 6 through the gap between the second support 4 and the permeation side chamber 2, and the leakage of gas from the space 6. Due to the holding portion 13, it is easy to place the second support body 4, the buffer body 5, and the thin film material 50. Further, the presence of the holding portion 13 can prevent the second support body 4, the buffer body 5, and the thin film material 50 from being displaced. Furthermore, since the holding portion 13 reduces the inflow of outside air and the outflow of gas from the gap, more accurate measurement can be performed.

  The first support 3 is fixed to a step portion 11 on the inner wall of the transmission side chamber 2 and a portion 9 having a second inner periphery. The first support 3 is fixed by, for example, an adhesive and cannot be detached. Moreover, the 1st support body 3 is closely_contact | adhered to the inner wall of the part 9 which has a 2nd inner periphery, and gas is not leaked from a clearance gap. In the first embodiment, the thickness of the first support 3 is equal to the height of the portion 9 having the second inner periphery.

The first support 3 has gas permeability. The gas permeability of the first support 3 is not particularly limited, but when the gas to be measured is, for example, water vapor, the water vapor permeability of the first support 3 is 1 × 10 ⁻¹⁵ mol / (m ^2. s · Pa) to 1 × 10 ⁻⁹ mol / (m ² · s · Pa), preferably 2 × 10 ⁻¹⁵ mol / (m ² · s · Pa) to 1 × 10 ^−9. mol ^/ more preferably ^(m 2 · s · Pa) or ^{less, 1 × 10 -14 mol / (} m 2 · s · Pa) or more at ^{1 × 10 -10 mol / (m} 2 · s · Pa) More preferably, it is 1 × 10 ⁻¹⁴ mol / (m ² · s · Pa) or more and 1 × 10 ⁻¹² mol / (m ² · s · Pa) or less. If the water vapor permeability is within this range, the inflow of water vapor can be more effectively reduced. In the first embodiment, the gas permeability between the thin film material 50 and the space 6 is adjusted by selecting the gas permeability of the second support 4. Therefore, the first support 3 has a higher gas permeability than the second support 4.

  The water vapor permeability of the first support 3 is obtained, for example, from the volume of the permeation side chamber 2 and the vacuum exhaust capacity and the time required for vacuum purification, or the volume of the permeation side chamber 2 and the gas to be measured. It can be selected by using a method obtained from the time required for cleaning by gas replacement without containing.

  The first support 3 preferably has a glass transition point of 100 ° C. or higher, more preferably 150 ° C. or higher, and further preferably 200 ° C. or higher. If the glass transition point is 100 ° C. or higher, it can withstand a heating operation (baking) for removing water vapor that is particularly troublesome to remove.

  Examples of the material of the first support 3 include an organic material and an inorganic material, and a composite material of an organic material and an inorganic material. Ceramics etc. are mentioned as an inorganic material. As organic materials, polycarbonate (glass transition point: about 145 ° C. to 150 ° C.), poly glass transition point glass transition point polyimide (about 285 ° C. to 420 ° C.), polyether ether ketone (about 143 ° C.), polyether sulfone (225) ° C), and polyamideimide (about 280-290 ° C). Note that the glass transition temperature largely depends on the molecular weight, composition, and manufacturing process, and thus may be selected based on the characteristics of each product regardless of the above.

  The thickness of the first support 3 is, for example, 1 mm or more and 20 mm or less, preferably 2 mm or more and 15 mm or less, and more preferably 5 mm or more and 10 mm or less.

  The 1st support body 3 plays the role which suppresses the leak of external air, and the role which suppresses the deformation | transformation of the sample by differential pressure | voltage.

  The second support 4 is detachably provided between the thin film material 50 and the first support 3. As shown in FIG. 2B, the second support 4 is in contact with the stepped portion 12 of the inner wall of the transmission side chamber 2, the inner wall of the portion 10 having the third inner periphery, and the first support 3. And held by the holding unit 13.

The second support 4 has gas permeability. The gas permeability of the second support 4 is lower than that of the first support 3. The gas permeability of the second support 4 is not particularly limited as long as it is lower than that of the first support 3. The gas permeability (for example, water vapor permeability) of the second support 4 is preferably ½ or less, more preferably 1/10 or less of the first support 3. When it is ½ or less of the first support 3, the supply-side chamber 1 and the permeation-side chamber 2 are evacuated or replaced with a gas that does not contain the gas to be measured until the gas permeability can be measured correctly. The time required for cleaning by can be further shortened. Moreover, when it is 1/10 or less of the 1st support body 3, the said time can further be shortened. When the gas to be measured is, for example, water vapor, the water vapor permeability of the second support 4 is 1 × 10 ⁻¹⁵ mol / (m ² · s · Pa) or more and 1 × 10 ⁻⁹ mol / (m ^2). S · Pa) or less, preferably 1 × 10 ⁻¹⁵ mol / (m ² · s · Pa) or more and 1 × 10 ⁻¹⁰ mol / (m ² · s · Pa) or less. It is preferably 1 × 10 ⁻¹⁴ mol / (m ² · s · Pa) or more and 1 × 10 ⁻¹⁰ mol / (m ² · s · Pa) or less, more preferably 1 × 10 ⁻¹⁴ mol / (1). and still further preferably in m ² · s · Pa) or more and ^{1 × 10 -12 mol / (m} 2 · s · Pa) or less. If the water vapor permeability is within this range, the water vapor permeability can be more appropriately controlled. In order to more accurately evaluate the gas permeability of the thin film material 50, the gas permeability of the support is preferably about 10 times higher than the gas permeability of the thin film material 50. In the present invention, the second support is used. The gas permeability between the thin film material 50 and the space 6 is adjusted by selecting the gas permeability of 4 according to the thin film material 50.

  Moreover, it is preferable that the 2nd support body 4 is higher than the temperature from which a glass transition point becomes the highest on a measurement, and it is more preferable that it is 100 degreeC or more. If the glass transition point is higher than the highest temperature in the measurement, it is possible to withstand a heating operation (baking) for removing water vapor that is particularly troublesome to remove.

Examples of the material of the second support 4 include an organic material and an inorganic material, and a composite material of an organic material and an inorganic material. Examples of organic materials include polystyrene (glass transition point: about 80 to 100 ° C.), polyethylene terephthalate (about 69 ° C.), polyethylene naphthalate (about 120 ° C.), cycloolefin polymer (about 100 to 160 ° C.), acrylic (70 ° C. Grade), polyacrylonitrile (about 104 ° C.), polytetrafluoroethylene (PTFE) (about 126 ° C.), and acrylonitrile butadiene styrene resin (about 80 to 125 ° C.). Further, SiOx these organic materials, SiNx, SiOxNy, composites with a deposit of an inorganic material such as _Al 2 _{O 3,} the composite material can be mentioned bonding the inorganic material to the organic material. Note that the glass transition temperature largely depends on the molecular weight, composition, and manufacturing process, and thus may be selected based on the characteristics of each product regardless of the above. Moreover, it is preferable to select a material in accordance with the temperature at which the temperature becomes the highest when performing gas permeability measurement.

  The thickness of the second support 4 is, for example, not less than 0.02 mm and not more than 2 mm, preferably not less than 0.05 mm and not more than 1 mm, and more preferably not less than 0.1 mm and not more than 0.5 mm.

  The buffer 5 is detachably provided between the thin film material 50 and the second support 4. As shown in FIG. 2B, the buffer body 5 is held by the holding portion 13 in a state where the buffer body 5 is in contact with the inner wall of the portion 10 having the third inner periphery and the second support body 4. The buffer 5 serves to reduce damage to the thin film material 50 due to contact between the second support 4 and the thin film material 50.

  The buffer 5 has gas permeability. The gas permeability of the buffer 5 is preferably higher than that of the second support 4. In the first embodiment, since the gas permeability between the thin film material 50 and the space 6 is adjusted to be more appropriate by selecting the second support 4, the gas permeability of the buffer 5 is the second. This is because a higher gas permeability can be maintained if it is higher than the support 4. Moreover, it is preferable that the durometer hardness (type A) of the buffer body 5 is 90-20. When the durometer hardness (type A) is within this range, damage to the thin film material 50 can be effectively reduced.

  Examples of the material of the buffer 5 include an organic material. Examples of organic materials include butadiene (durometer hardness (type A): about 60 to 70), chloroprene (about 37 to 90), styrene butadiene (about 46 to 69), nitrile (about 54 to 87), butyl (60 to 70). 70), ethylene propylene (about 41-90), chlorosulfonated polyethylene (about 57-69), acrylic (about 68), fluorine (about 80), silicone (about 50-70), urethane (about 50-90) ), Elastomers and rubber, soft polypropylene, soft polyethylene, soft polyvinyl chloride, and the like. The durometer hardness greatly depends on the molecular weight, the composition, and the manufacturing process. Therefore, the durometer hardness may be appropriately selected based on the characteristics of each product regardless of the above.

  The thickness of the buffer 5 is, for example, 0.02 mm or more and 3 mm or less, preferably 0.05 mm or more and 2 mm or less, more preferably 0.05 mm or more and 1 mm or less.

(Detector 21)
The detector 21 is not particularly limited as long as it is a conventionally known device capable of detecting the target gas. The types of known detectors 21 are various according to the detection principle, but can be appropriately selected according to the gas to be measured. The detector 21 is, for example, a mass analyzer, a dew point meter, a humidity sensor, a coulometric detector, a pressure sensor, a light absorption spectrometer, or a laser absorption spectrometer.

(Thin film material 50)
The thin film material 50 whose gas permeability is measured using the gas permeability measuring device 30 is, for example, a thin film glass film, a ceramic film, a surface thin film coating film such as a high barrier film for an organic EL device, a back sheet of a solar cell. Films used at high temperatures, such as films for foods, films for packaging foods, chemicals or electronic parts, and films for semiconductor materials. The thickness of the thin film material 50 is, for example, 0.02 mm or more and 2 mm or less.

  As described above, according to the gas permeability measuring device 30, when the thin film material 50 is set, the space 6 of the permeation side chamber 2 is not opened due to the presence of the first support 3, so that the outside air to the space 6 is not opened. Inflow can be suppressed. Therefore, it is possible to shorten the time for removing the gas to be measured from the gas permeable cell 20 before measuring the gas permeability of the thin film material 50. In particular, when measuring a plurality of thin film materials 50, it is not necessary to perform the above-described removal operation from scratch, which is more effective. Further, the removable second support 4 can be changed to one having an appropriate gas permeability according to the type of the thin film material 50 and the type of gas to be measured. Therefore, a plurality of thin film materials 50 having completely different gas permeability can be easily measured by the same gas permeability measuring device 30.

<Embodiment 2>
A second embodiment of the present invention will be described below with reference to FIG. FIG. 3 is a schematic diagram showing the configuration of the gas permeable cell 20 according to the second embodiment of the present invention. FIG. 3 shows a state in which the constituent members are assembled and the thin film material 50 to be measured is set.

  The gas permeation cell 20 includes a supply side chamber 1, a permeation side chamber 2, a second support 4, and a buffer 5. A supply port 14 is provided in the supply side chamber 1. The transmission side chamber 2 is provided with a discharge port 15 and a first support 3. Similarly to the first embodiment, the gas permeable cell 20 is a component of a gas permeability measuring device 30 (not shown) including a detector 21 (not shown).

  A configuration different from that of the first embodiment will be described below.

  The permeation side chamber 2 according to the second embodiment includes two portions having different inner peripheries, that is, a portion 8 having a first inner periphery, and a portion 9 having a second inner periphery larger than the first inner periphery. ,have. For this reason, the inner wall of the permeation side chamber 2 has a stepped portion 11 caused by the difference between the first inner periphery and the second inner periphery. The portion 9 having the second inner periphery forms a holding portion 13 for holding the second support body 4, the buffer body 5, and the thin film material 50.

  The first support 3 is fixed to a step portion 11 on the inner wall of the transmission side chamber 2 and a portion 9 having a second inner periphery. The first support 3 is fixed by, for example, an adhesive and cannot be detached. Moreover, the 1st support body 3 is closely_contact | adhered to the inner wall of the part 9 which has a 2nd inner periphery, and gas is not leaked from a clearance gap. In the second embodiment, the thickness of the first support 3 is smaller than the height of the portion 9 having the second inner periphery. The material and properties of the first support 3 are the same as those in the first embodiment.

  The second support 4 is detachably provided between the thin film material 50 and the first support 3. The second support 4 is held by the holding unit 13 in a state where the second support 4 is in contact with the inner wall of the portion 9 having the second inner periphery and the first support 3. The material and properties of the second support 4 are the same as those in the first embodiment.

  The buffer 5 is detachably provided between the thin film material 50 and the second support 4. The buffer body 5 is held by the holding unit 13 in a state where the buffer body 5 is in contact with the inner wall of the portion 9 having the second inner periphery and the second support body 4. The material and properties of the buffer 5 are the same as those in the first embodiment.

  Thus, in Embodiment 2, the 1st support body 3, the 2nd support body 4, the buffer body 5, and the thin film material 50 have the same area.

<Embodiment 3>
Embodiment 3 of the present invention will be described below with reference to FIG. FIG. 4 is a schematic diagram showing the configuration of the gas permeable cell 20 according to Embodiment 3 of the present invention. FIG. 4 shows a state in which the constituent members are assembled and the thin film material 50 to be measured is set.

  The gas permeation cell 20 includes a supply side chamber 1, a permeation side chamber 2, a second support 4, and a buffer 5. A supply port 14 is provided in the supply side chamber 1. The transmission side chamber 2 is provided with a discharge port 15 and a first support 3. Similarly to the first embodiment, the gas permeable cell 20 is a component of a gas permeability measuring device 30 (not shown) including a detector 21 (not shown).

  A configuration different from that of the first embodiment will be described below.

  The permeation side chamber 2 of Embodiment 3 includes two portions having different inner peripheries, that is, a portion 8 having a first inner periphery, and a portion 9 having a second inner periphery larger than the first inner periphery. ,have. For this reason, the inner wall of the permeation side chamber 2 has a stepped portion 11 caused by the difference between the first inner periphery and the second inner periphery. Unlike the first embodiment, the portion 9 having the second inner periphery does not have the holding portion 13 for holding the second support body 4, the buffer body 5, and the thin film material 50.

  The first support 3 is fixed to a step portion 11 on the inner wall of the transmission side chamber 2 and a portion 9 having a second inner periphery. The first support 3 is fixed by, for example, an adhesive and cannot be detached. Moreover, the 1st support body 3 is closely_contact | adhered to the inner wall of the part 9 which has a 2nd inner periphery, and gas is not leaked from a clearance gap. In the third embodiment, the thickness of the first support 3 is equal to the height of the portion 9 having the second inner periphery. The material and properties of the first support 3 are the same as those in the first embodiment.

  The second support 4 is detachably provided between the thin film material 50 and the first support 3. The second support 4 is placed in contact with the end surface of the portion 9 having the second inner periphery and the first support 3. The material and properties of the second support 4 are the same as those in the first embodiment.

  The buffer 5 is detachably provided between the thin film material 50 and the second support 4. The buffer 5 is placed in contact with the second support 4. The material and properties of the buffer 5 are the same as those in the first embodiment.

  As described above, in the third embodiment, the second support body 4, the buffer body 5, and the thin film material 50 are sandwiched between the supply side chamber 1 and the transmission side chamber 2 without being housed inside the transmission side chamber 2. It is.

<Other embodiments>
The numbers of supply ports and discharge ports in the supply side chamber 1 and the permeation side chamber 2 are not limited to those in the first to third embodiments. For example, in another embodiment, a discharge port 16 is provided in the supply-side chamber 1 as shown in FIG. 5A, and in another embodiment, as shown in FIG. As shown, a discharge port 16 is provided in the supply side chamber 1, and a supply port 17 is provided in the transmission side chamber 2.

  The permeation | transmission side chamber 2 is not limited to what has the level | step-difference part 11 (and level | step-difference part 12) like Embodiment 1-3. Therefore, in another embodiment, the first support 3 is not fixed to the step portion 11. For example, in another embodiment, as shown in FIG. 6A, the first support 3 is fixed to the inner wall of the transmission side chamber 2 that does not have a stepped portion. In FIG. 6A, the first support 3 is fixed to the outer peripheral portion thereof using, for example, pinning or screwing. In another embodiment, as shown in FIG. 6 (b), the first support 3 is not plate-shaped but has a shape in which feet are combined with plate-shaped portions. Is in contact with the inner wall (bottom) of the permeation side chamber 2. The end of the foot and / or the outer periphery of the foot and the plate-like portion are fixed to the inner wall of the permeation side chamber 2. The fixing is performed by, for example, an adhesive, pinning or screwing. In another embodiment, as shown in FIG. 6C, the first support 3 may be fixed to the inner wall via a base 18 that contacts the inner wall of the transmission side chamber 2. The stage 18 is provided such that one end thereof is in contact with the inner wall (bottom) of the transmission side chamber 2. And the 1st support body 3 is provided so that the other edge part of the stand 18 may be contact | connected. The stage 18 may be provided so as to be detachable from the transmission side chamber 2 or may be provided so as not to be detachable. Moreover, the stand 18 does not need to be a single component, and may be composed of a plurality of components.

  The first support 3 does not have to be fixed so as not to be removable with an adhesive or the like as in the first to third embodiments. For example, in another embodiment, the first support 3 is a permeation side chamber. 2 may be fixed detachably using bolts or the like. In such an embodiment, the first support 3 can be removed from the transmission side chamber 2 during repair or the like.

  The buffer body 5 is not an essential component, and in another embodiment, the gas permeable cell 20 does not include the buffer body 5.

  In Embodiments 1 to 3, the second support body 4 and the buffer body 5 are separate members, but the second support body 4 and the buffer body 5 may be an integral member. That is, in another embodiment, instead of the second support 4 and the buffer 5, the gas permeable cell 20 is formed by bonding the second support 4 and the buffer 5 or vapor-depositing one on the other. Equipped. Alternatively, in another embodiment, the gas permeable cell 20 includes the second support 4 that also serves as the buffer 5 instead of the second support 4 and the buffer 5. In this case, it is preferable that the durometer hardness (type A) of the 2nd support body 4 is 90-20.

  In the first to third embodiments, one each of the first support body 3, the second support body 4, and the buffer body 5 is provided, but a plurality of them may be provided. That is, in another embodiment, a plurality of first support bodies 3 are provided. In another embodiment, a plurality of second supports 4 are provided. In another embodiment, a plurality of buffer bodies 5 are provided.

  The shapes of the first support 3, the second support 4, and the buffer 5 may be plate-like as in the first to third embodiments, but are appropriate according to the shape of the thin film material 50. It is desirable.

  In addition, when the gas permeability is not measured, a lid may be installed on the first support 3, the second support 4, or the buffer 5, and a sealant (for example, beeswax) is provided around the lid. It may be sealed with. By covering, outside air can be prevented from entering the permeation side chamber 2 via the first support 3, the second support 4, and / or the buffer 5 while not in use.

[Article for measuring gas permeability]
The present invention is also an article used for measuring the gas permeability of the thin film material 50 and includes a permeation side chamber 2 provided with the first support 3 and a second support 4. Provide the goods. That is, the permeation side chamber 2 and the second support 4 can be provided as an article for measuring gas permeability for use in combination with an existing supply side chamber. The gas permeability measurement article may further include a buffer body 5. By using the article for measuring gas permeability in combination with the existing supply side chamber, the time for removing the target gas from the gas permeation cell before measuring the gas permeability of the thin film material 50 is shortened as compared with the conventional case. be able to.

  The present invention also provides an article used for measuring the gas permeability of the thin film material 50, which includes a second support 4 and a buffer 5. The article for measuring gas permeability is a candidate for selection according to the type of thin film material 50 and the type of gas to be measured. The gas permeability measurement article may include a plurality of second support bodies 4 and a plurality of buffer bodies 5.

  Note that various specific embodiments of the article for measuring gas permeability conform to the description in the above [Gas permeability measuring device] column.

[Gas permeability measurement method]
The gas permeability measuring method according to the present invention includes the steps of setting the thin film material 50 at a predetermined position of the gas permeability measuring device 30 and supplying the gas to be measured to the supply side chamber 1.

  The “predetermined position” means the surface of the buffer body 5 facing the second support body 4 when the buffer body 5 is included as a constituent element of the gas permeability measuring device 30. When not included as a component of the transmittance measuring device 30, it means on the surface of the second support 4 facing the first support 3.

  When the thin film material 50 is set at a predetermined position of the gas permeability measuring device 30, the second support 4, the buffer 5 (only when present), and the thin film material 50 are placed between the supply side chamber 1 and the permeation side chamber 2. Pinch. Thereafter, the periphery of the thin film material 50 may be sealed with a sealing material (for example, beeswax). Next, a gas that does not contain the gas to be measured is supplied from the supply port 14 to the supply side chamber 1, and the gas is discharged from the discharge port 15 of the transmission side chamber 2. As a result, the gas to be measured existing in the supply side chamber 1 and the permeation side chamber 2 is removed.

  Next, the gas to be measured is supplied to the supply side chamber 1 through the supply port 14. The gas supplied from the supply port 14 may be only the gas to be measured, or may be a mixed gas containing the gas to be measured. And the gas of the measuring object discharged | emitted from the discharge port 15 is quantitatively detected with the detector 21, and the gas permeability of the thin film material 50 is computed by a well-known method.

  The gas permeability measuring method according to the present invention may include a step of replacing the thin film material 50 and the second support 4 while the first support 3 is fixed to the inner wall of the permeation side chamber 2. In the gas permeability measurement method according to the present invention, it is preferable to select the second support 4 having a gas permeability of 100 to 100 times that of the thin film material 50 and 10000 times or less. By selecting a material in this range, the gas permeability between the thin film material 50 and the space 6 can be easily adjusted while the first support 3 is fixed.

  An example of a gas permeability measurement method according to the present invention will be described with reference to FIG. 1 assuming a case where the water vapor permeability of a plurality of thin film materials 50 having different water vapor permeability is measured. First, the second support 4 and the buffer 5 having water vapor permeability suitable for the first thin film material 50 are set in the permeation side chamber 2. As a setting method, the second support 4 is set on the permeation side chamber 2 and the first support 3, the buffer 5 is set on the second support 4, and the thin film material is set on the buffer 5. Set 50. For example, grease is applied and fixed between the permeation side chamber 2 and the second support 4, between the second support and the buffer 5, and between the buffer 5 and the thin film material 50. Then, for example, an O-ring and a gasket are set on the thin film material 50, and the second support body 4, the buffer body 5, and the thin film material 50 are firmly tightened between the supply side chamber 1 and the transmission side chamber 2. Next, a gas not containing water vapor is supplied from the supply port 14, and the gas is discharged from the discharge port 15. After the water vapor is sufficiently removed from the supply side chamber 1 and the permeation side chamber 2, water vapor or a gas containing water vapor is supplied from the supply port 14, and the water vapor discharged from the discharge port 15 is quantitatively detected by the detector 21. By detecting, the water vapor permeability of the first thin film material 50 is calculated by a known method.

  After the measurement of the water vapor transmission rate of the first thin film material 50 is completed, the supply-side chamber 1 is separated from the first thin film material 50, and the first thin film material 50, the buffer 5 and the second support 4 are moved. remove. Next, the second support 4 and the buffer 5 having water vapor permeability suitable for the second thin film material 50 are set in the permeation side chamber 2. At this time, the 1st support body 3 remains adhering to the inner wall of the permeation | transmission side chamber 2, and the space 6 is not open | released. The second thin film material 50 is set, and the second support 4, the buffer 5, and the second thin film material 50 are sandwiched between the supply side chamber 1 and the transmission side chamber 2. Next, a gas not containing water vapor is supplied from the supply port 14, and the gas is discharged from the discharge port 15. Here, since the space 6 was not opened when the thin film material 50 was replaced, water vapor contained in the atmosphere does not adhere to the transmission side chamber 2. Therefore, the water vapor removal time is greatly shortened.

  Thus, in the gas permeability measuring method according to the present invention, as described above, the first support 3 is not changed, and the second support 4 is matched with the thin film material 50 and has an appropriate gas permeability. Change to Therefore, the space 6 covered with the first support 3 is not opened when the thin film material is replaced, and the inflow of outside air is suppressed. Therefore, if the gas permeability measuring method according to the present invention is used, it is possible to shorten the time for removing the gas to be measured from the gas permeable cell 20 before measuring the gas permeability of the thin film material 50.

  The present invention can be used for gas permeability measurement of various thin film materials.

DESCRIPTION OF SYMBOLS 1 Supply side chamber 2 Permeation | transmission side chamber 3 1st support body (1st support body)
4 Second support (second support)
DESCRIPTION OF SYMBOLS 5 Buffer 6 Space 7 Space 8 Part which has 1st inner periphery 9 Part which has 2nd inner periphery 10 Part which has 3rd inner periphery 11 Step part 12 Step part 13 Holding part 14 Supply port 15 Discharge port 16 Discharge port 17 Supply port 18 units 20 Gas permeation cell 21 Detector (detection means)
30 Gas permeability measuring device 50 Thin film material

Claims (14)

An article used for measuring gas permeability of a thin film material,
A gas permeable first support fixed to the inner wall so as to cover at least a part of the space, and a permeation side chamber into which the gas that has permeated the thin film material flows;
Look including a second support member of low gas permeability gas permeability than the first support,
The second support is detachably provided between the thin film material and the first support,
The first support has a water vapor permeability of 2 × 10 ⁻¹⁵ mol / (m ² · s · Pa) to 1 × 10 ⁻⁹ mol / (m ² · s · Pa). The second support has a water vapor permeability of 1 × 10 ⁻¹⁵ mol / (m ² · s · Pa) or more and 1 × 10 ⁻¹⁰ mol / (m ² · s · Pa) or less,
The second support is an article for measuring gas permeability, wherein the gas permeability is ½ or less of that of the first support . The permeation side chamber has a portion having a first inner circumference and a portion having a second inner circumference larger than the first inner circumference,
The first support body is fixed to a step portion generated by a difference between the first inner periphery and the second inner periphery, and an inner wall of a portion having the second inner periphery. 1. The article for measuring gas permeability according to 1.   The article for gas permeability measurement according to claim 1 or 2, wherein the permeation side chamber has a holding part for holding the second support. The article for gas permeability measurement according to any one of claims 1 to 3 , wherein the first support has a glass transition point of 100 ° C or higher. The article for gas permeability measurement according to any one of claims 1 to 4 , wherein the permeation side chamber has a holding portion for holding the thin film material. The gas permeability measuring article according to any one of claims 1 to 5 , further comprising a gas permeable buffer body detachably provided between the thin film material and the second support. The article for gas permeability measurement according to claim 6 , wherein the permeation side chamber has a holding part for holding the buffer. The article for gas permeability measurement according to claim 6 or 7 , wherein the buffer has a durometer hardness (type A) of 90 to 20. The article for gas permeability measurement according to any one of claims 6 to 8 , wherein the buffer body has a gas permeability higher than that of the first support. The article for gas permeability measurement according to any one of claims 1 to 5 , wherein the second support has a durometer hardness (type A) of 90 to 20. It is a gas permeation cell used for measurement of gas permeability of a thin film material, Comprising: The article for gas permeability measurement of any one of Claims 1-10 , and the supply side to which the gas of measurement object is supplied from the outside A gas permeable cell comprising a chamber. A gas permeable cell according to claim 11 ;
A gas permeability measuring apparatus comprising: a detection unit configured to detect the measurement target gas that has passed through the thin film material from the supply side chamber and reached the transmission side chamber. A gas permeability measuring method, comprising: setting a thin film material at a predetermined position of the gas permeability measuring device according to claim 12 and supplying a gas to be measured to a supply side chamber. The gas permeability measurement method according to claim 13 , further comprising a step of replacing the thin film material and the second support while the first support is fixed to the inner wall of the permeation side chamber.

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