JP7550005B2 - Gas Permeability Measuring Device - Google Patents

Description

The present invention relates to a gas permeability measuring device.

For example, Patent Document 1 discloses a device that has a dedicated valve in the flow path from the test cell to the inspection section and adjusts the pressure inside the permeation tester by switching the dedicated valve.

Patent Document 2 also describes a gas permeability measuring device that includes a control unit that controls the operation of a vacuum pump and the opening and closing of valves between each process based on a signal from a pressure sensor.

Patent No. 6559147 JP2020-91108Publication

The gas permeability measuring devices described in Patent Documents 1 and 2 have the problem that the air pressure inside the device changes when the valve is switched depending on the flow rates of the detection gas and test gas, and the test temperature. Furthermore, the gas permeability measuring device disclosed in Patent Document 1 has the problem that it cannot be used when the test gas supply side is an open system.

In addition, the description in Patent Document 2 also includes a process of evacuating the inside of the cell, and does not disclose any gas permeability measuring device that can successfully suppress changes in air pressure caused by switching test gases, etc.

In light of these problems, there is a need for a new gas permeability measurement device that can effectively suppress sudden changes in air pressure within a cell used for measuring gas permeability and maintain high detection accuracy of the detection unit.

In order to solve the above problems, a gas permeability measuring device according to one embodiment of the present invention includes a first cell having a first recess that is blocked by a part of the sample when the sample is fixed therein during use, a test gas supply unit that supplies a test gas containing a target component to the sample from the outside of the first recess, a test gas exhaust unit that exhausts the test gas to the outside of the system, a detection gas supply unit that supplies a detection gas from the inside of the first recess to the target component that has permeated the sample, a detection gas exhaust unit having a flow path that exhausts the detection gas from the inside of the first recess to the outside of the system, a pressure reduction unit having a branch in the flow path that draws in a part of the detection gas from the branch, and a detection unit that detects the target component in the detection gas drawn in by the pressure reduction unit.

The gas permeability measuring device according to one embodiment of the present invention has the effect of successfully suppressing sudden changes in air pressure within a cell for measuring gas permeability, thereby maintaining high quantitative accuracy of the target component by the detection unit.

FIG. 1 is a diagram for explaining an outline of a gas permeability measuring device 100 according to one embodiment (first embodiment) of the present invention. FIG. 2 is a diagram for explaining an outline of an operation for attaching a sample to a first cell and a second cell in the gas permeability measuring device 100 according to one embodiment (first embodiment) of the present invention. FIG. 1 is a diagram for explaining an outline of a gas permeability measuring device 101 according to one embodiment (second embodiment) of the present invention. FIG. 13 is a diagram for explaining an outline of a gas permeability measuring device 102 according to one embodiment (third embodiment) of the present invention. FIG. 13 is a diagram for explaining an outline of a gas permeability measuring device 103 according to one embodiment (fourth embodiment) of the present invention.

<Gas permeability measuring device 100 (first embodiment)>
A gas permeability measuring device 100 according to one embodiment (first embodiment) of the present invention will be described in detail below with reference to Fig. 1. Fig. 1 is a diagram for explaining an outline of the gas permeability measuring device 100 according to this embodiment. As shown in Fig. 1, the gas permeability measuring device 100 includes a detection gas supply unit 20, a first cell 21, a detection gas discharge unit 22, a test gas supply unit 30, a second cell 31, a test gas discharge unit 32, a pressure reducing unit 40, and a detection unit 50. The gas permeability measuring device 100 also includes a cell storage unit 10, and the first cell 21 and the second cell 31 are detachably stored in the cell storage unit 10.

In FIG. 1, the second cell 31, the test gas supply unit 31, and the test gas exhaust unit 32 are arranged on the upper side of the paper of FIG. 1, and the first cell 21, the detection gas supply unit 21, the detection gas exhaust unit 22, the pressure reduction unit 40, and the detection unit 50 are arranged on the lower side of the paper of FIG. 1, but this is not limited to this. For example, the first cell 21 may be arranged above the second cell 31, or the first cell 21 and the second cell 31 may be arranged side by side.

2, in the gas permeability measuring device 100, the first cell 21 and the second cell 31 are arranged so that the opening of the first recess 21a and the opening of the second recess 31a face each other to sandwich the sample S, thereby fixing the sample S as shown in FIG. 1. This seals the opening of the first recess 21a and the opening of the second recess 31a with the sample S, preventing the test gas and the detection gas from directly mixing without permeating the sample S. In addition, in the gas permeability measuring device 100, the first cell 21 and the second cell 31 are stored in the cell storage section 10 with the sample S sandwiched between them. In addition, the first cell 21 and the second cell 31 may be fixed with the sample S sandwiched between them by an auxiliary fixing device (not shown).

As shown in FIG. 1, the gas permeability measuring device 100 has a detection gas supply unit 20, a first cell 21, and a detection gas exhaust unit 22 connected in this order to form a detection gas flow system, and the detection gas is sucked in from a branch 22b of the detection gas exhaust unit 22 by the pressure reducing unit 40, and a portion of the detection gas is sucked into the detection unit 50. In addition, the remaining detection gas that is not sucked in by the pressure reducing unit 40 but passes through the branch 22b and flows into the suction tube 22c is exhausted outside the system.

Similarly, as shown in FIG. 1, the gas permeability measuring device 100 has a test gas flow system in which the test gas supply section 30, the second cell 31, and the test gas exhaust section 32 are connected in this order so that they communicate with each other, and the gas is exhausted from the test gas exhaust section 32 to the outside of the system.

In the gas permeability measurement device, "outside the system" means that the detection gas discharged from the detection gas flow system and the test gas discharged from the test gas flow system mix with each other and do not affect the gas permeability measurement results, so long as this "outside the system" does not affect the gas permeability measurement results, the "outside the system" may be either inside or outside the gas permeability measurement device. In other words, in one embodiment of the gas permeability measurement device, the test gas and detection gas may be discharged either inside or outside the gas permeability measurement device, so long as the exhaust port for discharging the test gas and detection gas out of the system is "outside the system" that does not affect the gas permeability measurement results.

(Sample S)
The sample S, which is the object of measuring the gas permeability in the gas permeability measuring device 100 according to one embodiment of the present invention, is a sample formed into a film. The gas permeability measuring device 100 according to this embodiment can maintain the air pressure in the first recess 21a of the first cell 21 and the second recess 31a of the second cell 31 at substantially 1 atmosphere (standard atmospheric pressure), and can successfully suppress the air pressure from changing with the operation of the gas permeability measuring device 100. Therefore, according to the gas permeability measuring device 100 according to one embodiment of the present invention, the gas permeability can be accurately measured even in a thin-film sample, which is an example of a fragile sample that is at high risk of deformation or damage due to changes in the air pressure inside the cell in the gas permeability measuring device.

Such thin-film samples include, for example, barrier films for organic electronics, and film substrates for use in wearables and sensors. More specifically, examples include multilayer films in which layers of inorganic compounds such as metal oxides such as alumina, silica, and zirconia, or metal nitrides such as silicon nitride are formed on resin films such as polyethylene naphthalate (PEN), polyethylene terephthalate (PET), and polybutylene naphthalate (PBN), as well as resin films such as polyimide, acrylic, polyolefin, cycloolefin polymer, and polycarbonate. Such multilayer films may have multiple layers of inorganic compounds of different types on one resin film layer. Such thin-film samples have a problem in that the inorganic compound layers cannot fully follow the deformation of the resin film, resulting in damage and deformation, which reduces the accuracy of gas permeability measurement.

The gas permeability measuring device according to one embodiment of the present invention can accurately measure gas permeability, even for thin-film samples that are at high risk of deformation or damage due to changes in air pressure inside the cell.

(Detection Gas Supply Unit 20)
The detection gas supply unit 20 includes a detection gas storage unit 20a and a supply pipe 20b. The detection gas storage unit 20a may be a storage cylinder or a storage tank for the detection gas. The supply pipe 20b supplies the detection gas supplied from the detection gas storage unit 20a to the inside of the first recess 21a from a supply port provided inside the first recess 21a. In the example of FIG. 1, the detection gas is supplied by the detection gas supply unit 20 from the detection gas storage unit 20a through the supply pipe 20b in the direction of arrow A1 to the inside of the first recess 21a.

The volumetric flow rate of the detection gas per unit time in the detection gas supply unit may be determined taking into consideration the amount of detection gas sucked in per unit time by the detection unit (also referred to as the suction speed), which will be described later. The relationship between the amount of detection gas supplied per unit time by the detection gas supply unit (V), the amount of detection gas sucked in per unit time by the detection unit (V ₁ ), and the amount of detection gas discharged per unit time by the discharge unit (V ₂ ) satisfies the following formulas (1) to (3), all of which are expressed in units of "mL/min."
V= _V1 + _V2 ...(1)
V ₁ < V ≦ 1000, more preferably V ₁ + 10 ≦ V ≦ 500 (2)
V ₂ > 0, more preferably V ₂ ≧ 10, most preferably V ₂ ≧ 50... (3)
In the gas permeability measuring device 100, V ₁ in the above formula is the supply amount of the detection gas obtained in the supply tube 20b, V ₁ is the suction amount of the detection gas in the suction tube 22c, and V ₂ is the discharge amount of the detection gas in the discharge tube 22d. From the viewpoint of improving the quantitative accuracy of the target component in the detection unit, the volume flow rate V per unit time in the supply tube 20b of the detection gas is greater than the suction amount V ₁ of the detection gas per unit time in the suction tube, and more preferably is 10 mL/min or more greater than the suction amount V _1. In other words, the remainder obtained by subtracting the suction amount V ₁ from the volume flow rate V per unit time in the supply unit of the detection gas is discharged from the discharge unit as the discharge amount V ₂ , and the discharge amount V ₂ is more preferably 10 mL/min or more, and most preferably 50 mL/min or more. From the viewpoint of reducing the difference between the air pressure in the first recess and the air pressure in the second recess, the volumetric flow rate V per unit time in the supply pipe of the detection gas is more preferably 1000 mL/min or less, and more preferably 500 mL/min or less. The flow rate (supply amount) of the detection gas supplied from the detection gas storage unit 20a to the supply pipe 20b is measured by a flowmeter (not shown) provided in the supply pipe 20b, and the volumetric flow rate V of the detection gas may be detected by, for example, a mass flow controller, and the flow rate is manually or automatically controlled by a detection gas flow rate adjustment valve (not shown). Examples of the detection gas flow rate adjustment valve include a relief valve, a pressure reducing valve, a solenoid valve, a diaphragm valve, a needle valve, and a cylinder valve.

The inner diameter of the supply pipe 20b needs only to maintain the supply amount V of the detection gas per unit time described above, and may be appropriately designed using a known gas supply pipe.

The detection gas supplied by the detection gas supply unit 20 is a carrier gas that carries the target component (or, in some cases, the test gas and the target component) to the detection unit 50, and the carrier gas is not particularly limited as long as it is a gas that is inert to the target component. Examples of carrier gases include gases such as nitrogen, argon, helium, and oxygen.

In one embodiment of the gas permeability measurement device, the detection gas supply unit may include a plurality of detection gas storage units that separately store a plurality of types of detection gas, and a plurality of supply pipes that supply detection gas from each of the plurality of detection gas storage units into the first recess. This makes it more preferable that the gas permeability measurement device be able to appropriately select the detection gas depending on the type of sample and the type of target component.

(First cell 21)
The first cell 21 has a first recess 21a, and an opening of the first recess 21a is sealed on one side of the sample S. The first cell 21 has, inside the first recess 21a blocked by the sample S, a supply port for supplying the detection gas from the supply pipe 20b of the detection gas supply unit 20, and an exhaust port for exhausting the detection gas from the inside of the first recess 21a to the outside of the system.

Inside the first recess 21a, the target component permeates the sample S from the inside of the second recess 31a described below, as shown by arrow B2. Inside the first recess 21a, the detection gas supplied from the supply port via the supply pipe 20b captures the target component that has permeated the sample S, and is transported from the exhaust port to the exhaust pipe 22a in the direction of arrow A2, containing the target component.

In the gas permeability device 100 according to this embodiment, the air pressure in the first recess 21a is equal to the external air pressure outside the gas permeability device 100 and is maintained at substantially 1 atmosphere (standard atmospheric pressure). The first cell 21 having the first recess 21a is in communication with the detection gas exhaust section 22 that constantly exhausts the detection gas outside the system during a series of operations in the gas permeability measurement. For this reason, even if the type of detection gas supplied from the detection gas storage section 20a is switched, for example, the sudden change in air pressure in the first recess 21a caused by the switching of the detection gas can be suitably buffered. This makes it possible to suitably prevent damage and deformation of the sample S caused by the change in air pressure in the first recess 21a. Therefore, it is possible to suitably prevent the evaluation accuracy of the gas permeability in the sample S from decreasing due to the change in the permeability of the target component caused by the damage and deformation of the sample S. In addition, even if the amount of detection gas supplied into the first recess 21a is increased, the gas permeability device 100 can always discharge the detection gas from the discharge portion 22c, so that the air pressure in the first recess 21a can be prevented from increasing excessively. Therefore, in evaluating the gas permeability of a sample with high gas permeability, even if the amount of detection gas supplied is increased to increase the replacement efficiency of the detection gas in the first recess 21a, the air pressure in the first recess 21a can be prevented from increasing excessively. Therefore, by increasing the amount of detection gas supplied into the first recess 21a, the replacement efficiency of the detection gas can be increased, and this is one of the advantages of the present invention, which allows the gas permeability to be evaluated with high quantitative accuracy.

In addition, in one embodiment of the gas permeability measuring device, the first cell may be equipped with a heating unit (not shown), and the heating unit may heat the detection gas supplied into the first recess according to the gas permeability measurement conditions.

(Detection gas exhaust section 22)
The detection gas exhaust section 22 includes an exhaust pipe 22a and a branch (also called a branching section) 22b, which branches into an aspirating pipe 22c and an exhaust pipe 22d. The detection gas that has captured the target component inside the first recess 21a is exhausted to the exhaust pipe 22a along the direction of arrow A2 in Fig. 1, and a part of the detection gas containing the target component is aspirated along arrow A3 by the pressure reducing section 40 in the branch 22b. The remaining detection gas containing the target component is exhausted to the outside of the system from the exhaust pipe 22d along the direction of arrow 4A.

The volumetric flow rate passing through the exhaust pipe 22a is equal to the volumetric flow rate of the detection gas supplied in the supply pipe 20b, and the sum of the volumetric flow rate of the detection gas in the suction pipe 22c branching off at the branch 22b and the volumetric flow rate of the detection gas discharged outside the system by the exhaust pipe 22d is equal to the volumetric flow rate of the detection gas passing through the detection gas exhaust section 22a, or is equal when ignoring the amount of the target component that permeates into the first recess 21a.

The inner diameters of the suction pipe 22c and the exhaust pipe 22d may be appropriately designed using known piping as long as they can maintain the suction volume _V1 per unit time and the exhaust volume _V2 per unit time shown in the above formulas (1) to (3). The volumetric flow rate _V2 of the detection gas exhausted from the exhaust pipe 22d can be calculated from the volumetric flow rate V of the detection gas supplied from the supply pipe 20b of the detection gas supply unit 20 and the volumetric flow rate _V1 of the detection gas sucked into the detection unit 50 in the suction pipe 22c. In addition, a flow meter (not shown) for measuring the volumetric flow rate of the detection gas exhausted from the exhaust pipe 22c may be provided near the opening of the exhaust pipe 22c to the outside of the system.

(Pressure reduction section 40)
The pressure reducing section 40 may be realized by a pressure reducing pump such as a diaphragm pump, a dry pump, a scroll pump, a turbo molecular pump, and a rotary pump. The pressure reducing section 40 introduces the detection gas containing the target component passing through the branch 22b into the detection section 50 through the suction tube 22c. The pressure reducing section 40 generates an air pressure lower than the external air pressure (substantially 1 atmospheric pressure) of the gas permeability measuring device 100, and thus the detection gas is sucked in by the air pressure difference between the pressure reducing section 40 and the branch 22b. In addition, a flow meter (not shown) is provided in the suction tube 22c between the detection section 50 and the branch 22b, and the volumetric flow rate of the detection gas may be detected as the suction amount by, for example, a thermal mass flow meter, a micro-differential pressure sensor, a mass flow controller, or the like, and the flow rate is preferably manually or automatically controlled by an adjustment valve (not shown) that adjusts the suction amount _V1 so as to satisfy the following formulas (1) to (3) as the suction amount _V1 .
V= _V1 + _V2 ...(1)
V ₁ < V ≦ 1000, more preferably V ₁ + 10 ≦ V ≦ 500 (2)
V ₂ > 0, more preferably V ₂ ≧ 10, most preferably V ₂ ≧ 50... (3)

The pressure reducing section may be externally attached to the detection section or may be built in the detection section as long as it has a configuration for sucking in the detection gas containing the target component and allowing it to reach the detection section. The flow meter and the adjustment valve for adjusting the suction amount _V1 of the detection gas sucked into the detection section may be built in the detection section or may be provided in the piping that communicates between the detection section and the pressure reducing section. The suction amount _V1 of the detection gas may be controlled to be an appropriate suction amount depending on the type of the detection device that is the detection section 50.

(Detection Unit 50)
The detection unit 50 detects the target component in the detection gas that contains the target component that has permeated the sample S and reached the first cell 21. The detection unit 50 may be any one that can detect the target component carried by the detection gas, and a known detection means may be appropriately selected depending on the detection target. For example, when detecting water vapor as the target component, a known moisture meter may be used as the detection unit 50. Other examples of the detection unit 50 include detection devices such as atmospheric pressure ionization mass spectrometers, mass spectrometers, oxygen concentration meters, dew point meters, gas sensors, detector tubes, and infrared absorption spectrometers. The detection unit 50 may detect the target component by GC-MS (gas chromatography-mass spectrometry), HPLC (high performance (high pressure) liquid chromatography), and IC (ion chromatography).

The detection unit 50 may calculate the gas permeability obtained from the quantitative determination of the target component contained in the detection gas. The gas permeability obtained from the quantitative determination of the detection unit 50 may be selected according to the type of target component contained in the detection gas and the type of sample. For example, the permeability of water vapor is preferably calculated by a gas permeability measurement method conforming to JIS K7129-6:2019. One advantage of the gas permeability measurement device 100 is that it is possible to maintain the air pressure in the first cell at substantially 1 atmosphere even if the flow rate of the detection gas to the detection unit 50 is increased, and therefore it is possible to measure the gas permeability with high quantitative accuracy while maintaining the isobaric method.

Of course, the measurement of gas permeability is not limited to the gas permeability measurement method conforming to JIS K7129-6:2019, and may be appropriately determined according to the gas permeability measurement device 100 according to this embodiment, the gas permeability measurement devices 101, 102, and 103 according to other embodiments described later, and the types of sample and target component. For example, the gas permeability of the sample may be measured based on the flow rate of the detection gas, the gas concentration in the first cell that reached a steady state (a constant range regardless of time) during sample measurement, the gas concentration in the second cell before the test gas was introduced, etc., and at this time, various conditions such as temperature and air pressure during gas permeability measurement may be incorporated into the formula to measure. For example, the test gas is supplied to the second cell, and then the amount of the target component detected in the detection unit increases, and the amount of the target component contained in the detection gas is continuously measured until the numerical value becomes constant regardless of time and stabilizes, and the difference in numerical value before and after the introduction of the test gas is calculated from a numerical value converted into a specified unit. Alternatively, the test gas may be supplied to the second cell from the beginning, and the measurement may be terminated when the amount of the target component detected becomes constant and stable regardless of time, and the final value may be converted into a specified unit to determine the gas permeability.

In addition, unlike gas permeability measuring devices that first collect the target components contained in the detection gas in a collection tube and then introduce the collected target components into a gas detector for measurement, the gas permeability measuring device 100 has the advantage that it can make the intervals between the gas permeability plots finer, allowing for more precise gas permeability measurement. Therefore, a gas permeability measuring method using the gas permeability measuring device according to one embodiment of the present invention is also within the scope of the present invention.

(Test gas supply unit 30)
The test gas supply unit 30 includes a test gas storage unit 30a and a supply pipe 30b. The test gas storage unit 30a may be a storage cylinder or a storage tank for the test gas. The supply pipe 30b supplies the detection gas supplied from the test gas storage unit 30a to the inside of the second recess 31a from a supply port provided inside the second recess 31a. In the example of FIG. 1, the test gas is supplied by the test gas supply unit 30 from the detection gas storage unit 30a through the supply pipe 30b to the inside of the second recess 31a in the direction of the arrow B1.

Supply pipe 30b may have an inner diameter and cross-sectional area similar to those of supply pipe 20b, but is not limited thereto.

The volumetric flow rate per unit time in the supply pipe 30b of the test gas supplied by the test gas supply unit 30 may be designed to ensure sufficient quantitative accuracy of the target component and not to cause backflow from the exhaust pipe 32a, and is preferably approximately the same as the volumetric flow rate V of the detection gas supplied from the detection gas supply unit 20 to the first recess 21a. The flow rate (supply amount) of the test gas supplied from the test gas storage unit 30a to the supply pipe 30b is measured by a flow meter (not shown) provided in the supply pipe 30b, and the flow rate of the test gas may be detected, for example, by a mass flow controller, etc., and the flow rate is manually or automatically controlled by a test gas flow rate adjustment valve (not shown). The test gas flow rate adjustment valve can be a similar adjustment valve to the detection gas flow rate adjustment valve, so its description is omitted.

In one embodiment of the gas permeability measurement device, the test gas supply unit may include a plurality of test gas storage units that separately store a plurality of types of test gas, and a plurality of supply pipes that supply detection gas from each of the plurality of test gas storage units into the second recess. This makes it more preferable that the gas permeability measurement device be able to appropriately select the test gas depending on the type of sample and the type of target component.

(Second cell 31)
The second cell 31 has a second recess 31a on the inside, and an opening of the second recess 31a is blocked by a part of the sample S that blocks the opening of the first recess 21a and is exposed to the outside of the first recess 21a. The second cell 31 has, inside the second recess 31a blocked by the sample S, a supply port for supplying a detection gas from a supply pipe 30b provided in the test gas supply unit 30, and an exhaust port for exhausting the detection gas from the inside of the second recess 31a to the outside of the system.

The target component contained in the test gas supplied inside the second recess 31a permeates the sample S as shown by the arrow B3, and is captured by the detection gas inside the first recess 21a. The test gas supplied to the second recess 31a is discharged outside the system by the exhaust pipe 32a. In the gas permeability device 100 according to this embodiment, the air pressure inside the second recess 31a is equal to the air pressure outside the gas permeability device 100 and is substantially maintained at 1 atmosphere (standard atmospheric pressure). The second cell 31 having the second recess 31a is always connected to the test gas exhaust section 32 that discharges the test gas outside the system during a series of operations in the gas permeability measurement. For this reason, even if the type of test gas supplied from the test gas storage section 30a is switched, for example, the sudden change in air pressure inside the second recess 31a caused by the switching of the test gas can be suitably buffered. This makes it possible to suitably prevent damage and deformation of the sample S caused by the change in air pressure inside the second recess 31a. This effectively prevents a decrease in the evaluation accuracy of the gas permeability of the sample S due to changes in the permeability of the target component caused by damage and deformation of the sample S.

Test gases include gases that contain the target components to be measured. Examples of test gases include inorganic gases such as water vapor, oxygen, nitrogen, helium, hydrogen, argon, carbon dioxide, and carbon monoxide; organic gases such as methane; etc.

In addition, in one embodiment of the gas permeability measuring device, the second cell may be equipped with a heating unit (not shown), and the heating unit may heat the test gas supplied into the second recess according to the gas permeability measurement conditions.

(Test gas exhaust section 32)
The test gas exhaust section 32 includes an exhaust pipe 32a, and exhausts the test gas from the inside of the second recess 31a to the outside of the system along the direction of the arrow B2 in Fig. 1. This makes it possible to keep the inside of the second cell 31 within a preferable air pressure range even while the gas permeability measuring device 100 is in operation.

The volumetric flow rate of the test gas passing through the exhaust pipe 32a is equal to the volumetric flow rate of the test gas supplied in the supply pipe 30b, or is equal to the volumetric flow rate when the amount of the target component that permeates into the second recess 31a is ignored, and the test gas is always discharged from the exhaust pipe 32a during the measurement of the gas permeability. Note that a flow meter (not shown) for measuring the volumetric flow rate of the test gas discharged from the exhaust pipe 32a may be provided near the opening of the exhaust pipe 32a to the outside of the system.

[Control Unit]
The gas permeability measuring device according to one embodiment of the present invention may include a control unit. The control unit may, for example, control the amount of detection gas supplied by the detection gas supply unit, the amount of test gas supplied by the test gas supply unit, and the amount of detection gas suctioned by the detection unit and/or pressure reducing unit, and the amount of detection gas suctioned may be adjusted appropriately according to the specifications of the detection unit. The control unit may control the opening and closing of the adjustment valve in accordance with changes in the flow rate detected by the test gas flow sensor, the detection gas flow sensor, and the amount of detection gas suctioned as a volumetric flow rate, thereby controlling the flow rate of each gas, or may control the flow rate of each gas based on a preset timing chart.

<Gas permeability measuring device 101 (second embodiment)>
Hereinafter, one embodiment of the present invention (second embodiment) will be described in detail with reference to Fig. 3. Fig. 3 is a schematic diagram showing a gas permeability measurement device 101 according to this embodiment. As shown in Fig. 3, the gas permeability measurement device 101 includes a pressure control unit 60 in addition to the configuration of the gas permeability measurement device 100. The pressure control unit 60 includes a first pressure control unit 61, a second cell pressure control unit, and a second cell pressure control unit 62. In the gas permeability measurement device 101, the same members as those in the gas permeability measurement device 100 are designated by the same member numbers, and descriptions thereof will be omitted.

(Pressure control unit 60)
The pressure control unit 60 shown in Figure 3 includes a first pressure control unit 61 that controls the pressure in the first recess 21a of the first cell 21, and a second cell pressure control unit 62 that controls the pressure in the second recess 31a of the second cell 31.

The first pressure control unit 61 is provided with an air pressure sensor that detects the air pressure of the detection gas in the first recess 21a of the first cell 21, and an air pressure adjustment valve that adjusts the gas pressure of the detection gas in the exhaust pipe 22a. The second pressure control unit 62 is provided with an air pressure sensor that detects the air pressure of the test gas in the second recess 31a of the second cell 31, and an air pressure adjustment valve that adjusts the gas pressure of the test gas in the exhaust pipe 32a. That is, the first pressure control unit and the second pressure control unit only need to be provided with a device that has a barometer that detects air pressure as pressure and an air pressure adjustment valve that has an air pressure adjustment function, and an example of a device that has a barometer and an air pressure adjustment valve is a pressure switch. Examples of the barometer include sensors such as pressure sensors and pressure gauges, and examples of the air pressure adjustment valve for pressure control include relief valves, pressure reducing valves, solenoid valves, diaphragm valves, needle valves, and cylinder valves. Each of the air pressure adjustment valves provided in the first pressure control unit 61 and the second pressure control unit 62 is controlled manually or automatically. Moreover, the first pressure control unit 61 and the second pressure control unit 62 are preferably connected to each other by wire or wirelessly, and are equipped with a control unit (not shown) that can control the air pressure in the first recess 21a and the air pressure in the second recess 31a in conjunction with each other or individually.

With the above configuration, the gas permeability measuring device 101 can successfully measure gas permeability by the isobaric method in an atmospheric pressure environment in the detection unit 50 while adjusting the air pressure in the first recess 21a of the first cell 21 and the air pressure in the second recess 31a of the second cell 31. In addition, for example, it is also possible to measure the gas permeability of a film-like sample by setting a difference in air pressure between the first recess 21a and the second recess 31a within a range that does not damage the film-like sample.

Depending on the conditions for measuring the gas permeability, a film-like sample may be supported inside the first recess 21a and the second recess 31a by a support plate (not shown) made of a porous material, for example, and the gas permeability of the sample may be measured in this state.

<Gas permeability measuring device 102 (third embodiment)>
Hereinafter, an embodiment of the present invention (third embodiment) will be described in detail with reference to FIG. 4. FIG. 4 is a schematic diagram showing a gas permeability measurement device 102 according to this embodiment. As shown in FIG. 4, the gas permeability measurement device 102 can achieve the test gas supply section and the test gas discharge section by opening the cell storage section 10, instead of the test gas flow system including the test gas supply section 30, the second cell 31, and the test gas discharge section 32 of the gas permeability measurement device 100 shown in FIG. 1. In addition, in the gas permeability measurement device 102, the film-like sample S is fixed so as to be exposed in the cell storage section 10 by a sample fixing jig 70' having an opening area approximately equal to the opening area of the first recess 21a of the first cell 21. In the gas permeability measurement device 102, the first recess 21a is blocked by fixing the sample S by the sample fixing jig 70'.

That is, according to the gas permeability measuring device 102 of this embodiment, the surface of the sample S that does not face the first cell 21 can be suitably exposed to the outside air, and gas permeability measurement can be suitably performed under conditions of substantially 1 atmosphere. That is, it is also possible to compare the gas permeability measurement results when the sample S is tested without exposing it to the atmosphere, using the outside air as the test gas. Since the pressure inside the first cell 21 is controlled to atmospheric pressure, the risk of deformation or damage of the sample S can also be reduced in the gas permeability measuring device 102 of this embodiment. That is, since the air pressure of the first cell can be maintained at substantially 1 atmosphere, the sample S can be exposed to the atmosphere outside the gas permeability measuring device 102 by the isobaric method for testing.

<Gas Permeability Measuring Device 103 (Fourth Embodiment)>
Hereinafter, one embodiment of the present invention (fourth embodiment) will be described in detail with reference to Fig. 5. Fig. 5 is a diagram for explaining an outline of a gas permeability measurement device 103 according to this embodiment. As shown in Fig. 5, the gas permeability measurement device 103 has a configuration in which a sample fixing jig 70 is added to the gas permeability measurement device 100.

As shown in FIG. 5, the sample fixing jig 70 has a first surface 71 facing the first cell, a second surface 72 facing the second cell, and an opening that penetrates from the first surface 71 to the second surface 72. The sample fixing jig 70 fixes the sample S so that it blocks the opening and is exposed to both the first surface 71 side and the second surface 72 side.

The sample fixing jig 70 may be a known fixing jig with any configuration depending on the type and shape of the sample S'. With this configuration, the first cell 21 and the second cell 31 can be used to measure a sample S of any shape, regardless of the shape of the sample.

More specifically, the sample fixing jig 70 may be made of a material that has a lower gas permeability than the sample, such as metal and ceramics. There are no limitations on the type of sample S' as long as it can be fixed to the sample fixing jig 70, and examples of samples include medical instruments such as syringes and organic EL devices.

The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope of the claims. The technical scope of the present invention also includes embodiments obtained by appropriately combining the technical means disclosed in different embodiments.

〔summary〕
A gas permeability measuring device according to one embodiment of the present invention comprises a first cell having a first recess which is blocked by a portion of the sample when the sample is fixed therein during use, a test gas supply section which supplies a test gas containing a target component to the sample from the outside of the first recess, a test gas exhaust section which discharges the test gas to the outside of the system, a detection gas supply section which supplies a detection gas from the inside of the first recess to the target component which has permeated the sample, a detection gas exhaust section having a flow path which discharges the detection gas from the inside of the first recess to the outside of the system, a pressure reduction section having a branch in the flow path which draws in a portion of the detection gas from the branch, and a detection section which detects the target component in the detection gas drawn in by the pressure reduction section.

In addition, a gas permeability measuring device according to one embodiment of the present invention may include a second recess, a second cell to which the test gas is supplied from the test gas supply unit to the inside of the second recess, and a test gas exhaust unit that exhausts the test gas supplied to the inside of the second recess to the outside of the system, and the sample may be fixed so that a part of the sample exposed to the outside of the first recess covers the second recess.

Moreover, it is more preferable that the gas permeability measuring device according to one embodiment of the present invention is provided with a pressure control unit that controls the pressure inside the first cell midway from the inside of the first recess in the detection gas discharge section to the branch.

Moreover, it is more preferable that the gas permeability measuring device according to one embodiment of the present invention is provided with a pressure control unit that controls the pressure inside the first cell on the way from the inside of the first recess in the detection gas discharge section to the branch, and controls the pressure inside the second cell on the way from the inside of the second recess in the test gas discharge section to the outside of the system.

In addition, in the gas permeability measuring device according to one embodiment of the present invention, the sample may be a film.

The gas permeability measuring device according to one embodiment of the present invention may also include a sample fixing tool that has a first surface that covers the first recess, a second surface that covers the second recess, and an opening that penetrates from the first surface to the second surface, and that fixes the sample so that the opening is blocked by the sample and the sample is exposed to both the first surface side and the second surface side. This makes it possible to perform measurements using the gas permeability measuring device according to this embodiment regardless of the shape of the sample.

The present invention can be used in a wide range of fields that require the measurement of gas permeability, including food, medicine, organic electroluminescence devices, and solar cells.

100: Gas permeability measuring device 101: Gas permeability measuring device 102: Gas permeability measuring device 103: Gas permeability measuring device 20: Detection gas supply unit 21: First cell 21a: First recess 22: Detection gas exhaust unit 22a: Branch 30: Test gas supply unit 31: Second cell 31a: Second recess 32a: (Test gas exhaust unit)
40: Pressure reducing section 50: Detection section 60: Pressure control section 61: First pressure control section 62: Second pressure control section 70: Sample fixing jig 70': Sample fixing jig 71: First surface 72: Second surface S: Sample S': Sample

Claims (5)

a first cell having a first recess, the first recess being blocked by a part of the sample when the sample is fixed therein during use;
a test gas supply unit that supplies a test gas containing a target component to the sample from outside the first recess;
a test gas exhaust section that exhausts the test gas to the outside of the system;
a detection gas supply unit that supplies a detection gas to the target component that has permeated the sample from the inside of the first recess;
a detection gas exhaust unit having a flow path for exhausting the detection gas from the inside of the first recess to the outside of the system;
a pressure reducing section having a branch in the flow path, the pressure reducing section sucking a part of the detection gas from the branch through a suction tube;
a detection unit that detects the target component in the detection gas sucked by the pressure reducing unit ,
The gas permeability measuring device further comprises a pressure control section for controlling the pressure inside the first cell, midway from the inside of the first recess in the detection gas discharge section to the branch . A second cell including a second recess, the test gas being supplied from the test gas supply unit to the inside of the second recess;
a test gas exhaust section that exhausts the test gas supplied to the inside of the second recess to the outside of the system;
2. The gas permeability measuring device according to claim 1, wherein the sample is fixed so that a part of the sample exposed outside the first recess covers the second recess. a first cell having a first recess, the first recess being blocked by a part of the sample when the sample is fixed therein during use;
a test gas supply unit that supplies a test gas containing a target component to the sample from outside the first recess;
a test gas exhaust section that exhausts the test gas to the outside of the system;
a detection gas supply unit that supplies a detection gas to the target component that has permeated the sample from the inside of the first recess;
a detection gas exhaust unit having a flow path for exhausting the detection gas from the inside of the first recess to the outside of the system;
a pressure reducing section having a branch in the flow path, the pressure reducing section sucking a part of the detection gas from the branch through a suction tube;
a detection unit that detects the target component in the detection gas sucked by the pressure reducing unit;
A second recess;
a second cell to which the test gas is supplied from the test gas supply unit to an inside of the second recess;
a test gas exhaust section that exhausts the test gas supplied to the inside of the second recess to the outside of the system;
Fixing the sample such that a portion of the sample exposed outside the first recess covers the second recess ;
a pressure inside the first cell is controlled on a path from an inside of the first recess in the detection gas discharge portion to the branch;
a pressure control section for controlling the pressure inside the second cell on the way from the inside of the second recess in the test gas discharge section to the outside of the system. The gas permeability measuring device according to any one of claims 1 to 3 , wherein the sample is a film. a first surface that closes the first recess, a second surface that closes the second recess, and an opening that penetrates from the first surface to the second surface;
4. The gas permeability measuring device according to claim 2, further comprising a sample fixing jig for fixing the sample so that the sample closes the opening and the sample is exposed to both the first surface side and the second surface side.

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