WO2015041115A1 - Gas permeability measuring device - Google Patents

Gas permeability measuring device Download PDF

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Publication number
WO2015041115A1
WO2015041115A1 PCT/JP2014/073925 JP2014073925W WO2015041115A1 WO 2015041115 A1 WO2015041115 A1 WO 2015041115A1 JP 2014073925 W JP2014073925 W JP 2014073925W WO 2015041115 A1 WO2015041115 A1 WO 2015041115A1
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Prior art keywords
gas
measurement
barrier film
calibration
unit
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PCT/JP2014/073925
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French (fr)
Japanese (ja)
Inventor
吉田　肇
高橋　善和
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独立行政法人産業技術総合研究所
株式会社Ｔｉ
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Application filed by 独立行政法人産業技術総合研究所, 株式会社Ｔｉ filed Critical 独立行政法人産業技術総合研究所
Priority to JP2015537875A priority Critical patent/JP6281915B2/en
Publication of WO2015041115A1 publication Critical patent/WO2015041115A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082—Investigating permeability by forcing a fluid through a sample
    • G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change

Definitions

  • the present invention relates to a gas permeability measuring apparatus having a measuring unit for measuring the gas permeability of a gas barrier film and a calibration unit for calibrating the measuring unit.
  • Gas barrier films are expected to play an important role in various fields such as the packaging field for food, medicine, electronic parts, etc., and the sealing field for electronic parts. Since the gas barrier film is used according to its gas barrier properties, that is, gas permeability, the accurate measurement of the gas permeability of the gas barrier film is extremely important for the role. It becomes.
  • an apparatus for measuring the gas permeability of the gas barrier film for example, a flange for holding the film, a container for exposing the gas to the film, and a gas permeation on the opposite side of the gas exposure surface of the film
  • a vacuum unit capable of exhausting to a predetermined pressure with respect to the surface is connected, and the gas permeability of the gas permeating from the gas transmission surface into the vacuum unit is measured by a mass spectrometer attached to the vacuum unit
  • An apparatus has been proposed (see Patent Document 1).
  • the apparatus does not have means for calibrating the mass spectrometer, in order to calibrate the mass spectrometer, it is necessary to remove the mass spectrometer from the apparatus and calibrate it using an appropriate calibration means. There is. In this case, not only the calibration work becomes complicated, but also the sensitivity of the mass spectrometer depends on the reproducibility associated with the removal / transport / installation work, the environmental conditions (temperature, etc.) during calibration and measurement, and the difference in installation orientation. The characteristics may change, and accurate measurement of gas permeability may not be possible. Further, since the gas flow path system for calibration to which the mass spectrometer is attached is different from the gas flow path system of the apparatus, the mass spectrometer calibrated with the gas flow path system for calibration is used. When the gas permeability in the gas flow path system of the apparatus is measured, the calibration cannot reflect the flow rate of the gas in the gas flow path system of the apparatus, and the gas permeability of the gas barrier film cannot be accurately measured There is.
  • an object of the present invention is to provide a gas permeability measuring apparatus capable of simplifying the calibration operation without removing the gas permeability measuring unit and accurately measuring the gas permeability.
  • Means for solving the problems are as follows. That is, ⁇ 1>
  • the gas barrier film holding portion disposed on the gas exposure surface side of the gas barrier film and the gas permeation side holding portion disposed on the gas permeation surface side of the gas barrier film sandwich and hold the peripheral portion of the gas barrier film.
  • the gas exposure chamber defined by the gas exposure surface into which the measurement gas flows and the gas exposure side holding portion, and the gas transmission surface transmit the gas barrier film.
  • a film holding chamber in which a gas permeation chamber defined by the gas permeation surface into which the measurement gas is introduced and the gas permeation side holding portion is formed, a gas supply portion for supplying the measurement gas, An openable and closable measurement channel disposed between a gas supply unit and the gas exposure side holding unit, and a measurement channel disposed between the gas supply unit and the gas exposure side holding unit, wherein the measurement channel is closed.
  • the flow rate of the measurement gas flowing out from the film holding chamber in a state where the gas barrier film is not held can be calibrated and measured by the calibration measuring unit, and the gas permeation can be performed while the gas barrier film is held.
  • the measurement gas is caused to flow out from the gas permeation-side holding portion along the inflow direction of the measurement gas flowing into the film holding chamber, and the vacuum portion is hollow along the inflow direction.
  • the gas permeability measuring device according to ⁇ 1>, wherein a vacuum pump is disposed at an extended position of the gas pump.
  • a calibration measurement unit is formed of at least one of an orifice, a thin tube, and a porous body, and a conductance unit whose conductance is measured in advance, and a pressure for measuring the pressure of the measurement gas flowing into the conductance unit
  • the gas permeability measuring device according to any one of ⁇ 1> to ⁇ 2>, further including a measuring unit.
  • the gas permeability measuring device according to ⁇ 3>, wherein the conductance part can flow the measurement gas in a state where the molecular flow condition is satisfied.
  • a transmittance measuring device can be provided.
  • FIGS. 1 (a) and 1 (b) An embodiment of the gas permeability measuring apparatus of the present invention will be described with reference to FIGS. 1 (a) and 1 (b).
  • Fig.1 (a) is explanatory drawing which shows the outline
  • FIG.1 (b) is explanatory drawing which shows the outline
  • the gas permeability measuring device 1 includes a film holding chamber 10, a gas upstream portion 20, and a gas downstream portion 40.
  • the film holding chamber 10 includes a gas exposure side holding portion 11 disposed on the gas exposure surface side of the gas barrier film 2 and a gas permeation side holding portion disposed on the gas transmission surface side opposite to the gas exposure surface of the gas barrier film 2. 13.
  • the gas exposure side holding part 11 and the gas permeation side holding part 13 are arranged to face each other with the gas barrier film 2 interposed therebetween, and can be held by holding the peripheral part of the gas barrier film 2. When the gas barrier film 2 is held (see FIG.
  • the gas exposure chamber A defined by the gas exposure surface into which the measurement gas flows and the gas exposure side holding unit 11 are formed
  • the gas permeation A gas permeation chamber B defined by the gas permeation surface into which the measurement gas permeating from the surface flows and the gas permeation side holding portion 13 is formed.
  • the gas exposure side holding part 11 and the gas permeation side holding part 13 are large enough that the gas barrier film 2 is exposed to a sufficient amount of the measuring gas in the gas exposure chamber A and the gas permeation chamber B, and the permeation amount can be measured.
  • gas exposure side holding part 11 and the gas permeation side holding part 13 have seal members 12, 14 such as O-rings in order to maintain the gas tightness of the gas exposure chamber A and the gas permeation chamber B.
  • seal members 12, 14 such as O-rings in order to maintain the gas tightness of the gas exposure chamber A and the gas permeation chamber B.
  • the peripheral part of the gas barrier film 2 is sandwiched between 12 and 14 and held.
  • the film holding chamber 10 covers the outside of the seal members 12 and 14 and forms an exhaust chamber C in order to eliminate leak gas that enters the gas exposure chamber A and the gas permeation chamber B from between the seal members 12 and 14. You may have the exhaust part 15 to do. In this case, the gas in the exhaust chamber C is exhausted by operating the vacuum pump 17 with the on-off valve 16 open. In the state where the gas barrier film 2 is not held (FIG. 1A), the film holding chamber 10 can form an airtight space defined by the gas exposure side holding part 11 and the gas permeation side holding part 13. It is said.
  • the gas upstream section 20 includes gas supply sections 21 and 22 that supply the measurement gas, and an openable and closable measurement flow path 25 that is disposed between the gas supply sections 21 and 22 and the gas exposure side holding section 11.
  • the calibration flow path 27 is arranged between the gas supply units 21 and 22 and the gas exposure side holding unit 11.
  • the gas supply units 21 and 22 supply the measurement gas to the measurement flow path 25 or the calibration flow path 27 with the on-off valves 23 and 24 being opened.
  • gas supply parts 21 and 22 any one may be sufficient and you may have three or more.
  • the measurement gas can be appropriately selected according to the purpose of measuring the gas permeability with respect to the gas barrier film 2.
  • the measurement channel 25 has an open / close valve 26 in the channel, and transfers the measurement gas supplied from the gas supply units 21 and 22 to the gas exposure side holding unit 11.
  • the calibration flow path 27 has an open / close valve 29 in the flow path, and transfers the measurement gas supplied from the gas supply units 21 and 22 to the gas exposure side holding unit 11.
  • the calibration flow path 27 is used when the film holding chamber 10 does not hold the gas barrier film 2 (FIG. 1A), and is opened when the measurement flow path 25 is closed.
  • the measurement channel 25 is used in a state where the film holding chamber 10 holds the gas barrier film 2 (FIG. 1B). When the measurement channel 25 is opened, the calibration channel 27 is used. Is closed.
  • one of the flow paths is opened in a state where the gas barrier film 2 is not held and a state where the gas barrier film 2 is held, and the measurement gas supplied from the gas supply units 21 and 22 is supplied to the gas exposure side. Transfer to the holding unit 11.
  • one end side is connected to the measurement flow path 25 and the calibration flow path 27, and an exhaust flow path for exhausting the measurement flow path 25 and the calibration flow path 27 is arranged before measuring the gas permeability. May be.
  • the other end side of the exhaust passage can be connected to the vacuum pump 17 so that the inside of the measurement passage 25 and the calibration passage 27 can be exhausted.
  • the calibration flow path 27 has a calibration measurement unit that measures the flow rate of the measurement gas that flows into the film holding chamber 10 in the open state without holding the gas barrier film 2.
  • the specific configuration of the calibration measuring unit is not particularly limited, but from the viewpoint of accurately measuring the diversion of the measuring gas, the calibration measuring unit is configured by at least one of an orifice, a thin tube, and a porous body and circulates. It is preferable to include a conductance unit 28 in which the gas conductance is measured in advance, and a pressure measurement unit 30 that measures the pressure of the measurement gas flowing into the conductance unit 28.
  • the conductance portion 28 may be configured by combining an orifice, a thin tube, and a porous body.
  • a microporous filter described in JP 2011-47855 A can be suitably used as the porous body.
  • a pressure measuring unit 30 a known pressure gauge or the like can be used, but a pressure gauge (such as a diaphragm vacuum gauge) whose characteristics do not change depending on the type of gas is preferably used.
  • a hygrometer may be installed.
  • the measurement gas can be circulated in a state where the conductance part 28 satisfies the molecular flow condition.
  • the difference in conductance due to the type of gas can be corrected only by the molecular weight, and the interaction of each gas type in the mixed gas can be eliminated.
  • the flow rate and flow rate ratio of the mixed gas flowing out from the conductance unit 28 can be obtained.
  • the pressure of the mixed gas supplied to the conductance unit 28 can be controlled within a predetermined range.
  • the gas permeability measuring apparatus 1 it is possible to calibrate (without removing) the gas permeability measuring unit 43 regardless of the gas configuration and gas type of pure gas or mixed gas, and the obtained calibration result On the basis of the above, the gas permeability of the measuring gas composed of these to the gas barrier film 2 can be accurately measured.
  • the gas downstream portion 40 includes a hollow vacuum portion 41 connected to the gas permeation side holding portion 13, a vacuum pump 42 that exhausts the inside of the vacuum portion 41, and a gas permeability measurement portion 43 attached to the vacuum portion 41. Is done.
  • the vacuum part 41 can be constituted by a known vacuum container, and it is preferable that the pressure can be evacuated to 10 ⁇ 4 Pa or less in consideration of measurement with respect to a high barrier film.
  • a known pump such as a diffusion pump, a turbo molecular pump, a cryopump, a sputter ion pump, and a getter pump can be used as the vacuum pump 17.
  • the vacuum pump 42 is preferably used for high vacuum or ultra-high vacuum in order to keep the pressure in the vacuum part 41 low.
  • the gas permeability measurement unit 43 can measure the flow rate of the measurement gas flowing out from the film holding chamber 10 in a state where the gas barrier film 2 is not held (FIG. 1A) by the calibration measurement unit. In addition, the flow rate of the measurement gas that has permeated the gas barrier film 2 flowing out from the gas permeation chamber B in a state where the gas barrier film 2 is held (FIG. 1B) can be calibrated and measured by the calibration measurement unit. Is done.
  • a known vacuum gauge such as an ionization vacuum gauge or a known mass spectrometer such as a quadrupole mass spectrometer can be used.
  • the gas permeability measuring apparatus 1 is configured to cause the measurement gas to flow out from the gas permeation-side holding unit 13 along the inflow direction of the measurement gas flowing into the film holding chamber 10, and the vacuum unit 41 includes the vacuum unit 41. It is hollow along the inflow direction, and the vacuum pump 42 is arranged at an extended position in the inflow direction. By being configured in this way, the measurement gas flowing into the film holding chamber 10 flows out from the gas permeation-side holding unit 13 without partial deviation, and the outflowed measurement gas flows. It is possible to eliminate partial deviation in the vacuum part 41, and the gas permeability measuring part 43 can measure the flow rate of the measuring gas with a stable behavior.
  • the measurement gas supplied from the gas supply units 21 and 22 is passed through the calibration channel 27 without holding the gas barrier film 2 (FIG. 1A). Then, the gas is allowed to flow into the film holding chamber 10, and the flow rate thereof can be measured by the gas permeability measuring unit 43. That is, the flow rate of the measurement gas flowing out from the conductance unit 28 constituting the calibration measurement unit in the calibration channel 27 is calculated from the pressure measured by the pressure measurement unit 30, the conductance and temperature of the conductance unit 28. By correlating the flow rate with the indicated value of the gas permeability measuring unit 43, the indicated value of the gas permeability measuring unit 43 corresponding to the flow rate of the measuring gas flowing into the film holding chamber 10, and then the vacuum part 41, is obtained. A calibration curve can be created.
  • the measurement gas supplied from the gas supply units 21 and 22 flows into the gas exposure chamber A of the film holding chamber 10 through the measurement channel 25.
  • the gas permeability measuring unit 43 can measure the flow rate of the measurement gas (permeated gas) that passes through the gas barrier film 2 and flows out of the gas permeation chamber B. That is, based on the calibration curve obtained without holding the gas barrier film 2 (FIG. 1A), the flow rate of the measuring gas (permeating gas) corresponding to the indicated value of the gas permeability measuring unit 43 is obtained. be able to.
  • the gas permeability measuring apparatus 1 since the calibration flow path 27 having the calibration measuring section for calibrating the gas permeability measuring section 43 is arranged in the apparatus, the gas permeability is measured one by one.
  • the measuring device 43 can be removed from the device and calibrated. After the calibration, the work of attaching to the device can be omitted, and the calibration work can be simplified. Further, by providing the calibration flow path 27 having the calibration measurement section in the gas upstream section 20, the gas of the measurement gas flowing into the film holding chamber 10 from the calibration flow path 27 and the measurement flow path 25. Since the flow path to the permeability measuring unit 43 is the same (refer to the arrows indicating the gas flow paths in FIGS.
  • the gas permeability measuring unit 43 is used for the measurement at the time of calibration.
  • Gas measurement conditions can be made common with those at the time of measurement, and high reliability is ensured for the indicated value of the gas permeability measurement unit 43 at the time of calibration. Therefore, the gas permeability measuring apparatus 1 can measure an accurate gas permeability at the time of measurement based on a highly reliable calibration curve created at the time of calibration.
  • the calibration unit is provided in the apparatus, a configuration in which only the measurement channel 25 is arranged in the gas upstream unit 20 and the calibration channel 27 is arranged in the vacuum unit 41 of the gas downstream unit 40 is also considered.
  • the flow path of the measurement gas that flows into the film holding chamber 10 to the gas permeability measurement unit 43 differs between the calibration time and the measurement time. Changes occur in the pressure distribution and the direction distribution of flying gas molecules. Therefore, under the influence of the difference in the flow conditions of the measurement gas, the reliability of the measurement result of the gas permeability measured at the time of measurement is lowered based on the calibration curve created at the time of calibration.
  • the gas permeability measuring apparatus 1 illustrates one embodiment of the present invention, and the technical idea of the present invention is not limited to this as long as the above-described effects are exhibited.
  • a gas permeability measurement method using the gas permeability measuring apparatus 1 will be described as an example together with an actual measurement example. That is, a measurement method and measurement when gas permeability is measured using a gas permeability measuring device configured in accordance with the gas permeability measuring device 1 described above (see FIGS. 1A and 1B). The results will be described. In the following, for convenience of explanation, the measurement method and the measurement results will be described using the same reference numerals as those of the gas permeability measuring apparatus 1.
  • the vacuum pumps 17 and 42 are operated to evacuate the inside of the gas permeability measuring device 1.
  • the measurement values of the pressure measurement unit 30 and the gas permeability measurement unit 43 in this state are recorded as zero points.
  • the on-off valve 26 of the measurement channel 25 closed and the on-off valve 29 of the calibration channel 27 opened the on-off valve 23 of the gas supply unit 21 is opened to supply the measurement gas from the gas supply unit 21.
  • the measurement gas flows into the film holding chamber 10 from the gas exposure side holding unit 11 side through the calibration channel 27 and flows out from the gas permeation side holding unit 13 side to the vacuum unit 41.
  • the pressure measurement unit 30 and the gas permeability measurement unit 43 wait for the measurement values to become constant, and the pressure measurement unit 30 measures the pressure before the conductance unit 28 flows into the measurement gas. Information on the flow rate of the measurement gas that has flowed out is measured. The measurement was performed using water vapor as the measurement gas, and using an ionization vacuum gauge and a quadrupole mass spectrometer as the gas permeability measurement unit 43.
  • the pressure before the conductance part 28 inflow measured by the pressure measurement part 30 adjusts the supply amount of the measurement gas from the gas supply part 21, and thereby the flow of the measurement gas flowing through the conductance part 28 Can be controlled to satisfy the molecular flow condition.
  • the flow rate Q s (Pa ⁇ m 3 / s) of the measurement gas flowing through the conductance part 28 and flowing out to the vacuum part 41 via the film holding chamber 10 is expressed by the following formula (1). expressed.
  • P R represents the pressure minus the zero point from the measured values of the pressure measuring unit 30
  • C s is the conductance portion 28 measured in advance typical gas (here in, a molecular flow conductance in nitrogen gas)
  • M N2 represents the molecular weight of nitrogen
  • M represents a molecular weight of the measuring gas (water vapor)
  • T 0 represents the temperature at C s measurement
  • T indicates the temperature of the gas supply unit 21 when the measurement gas is supplied.
  • the flow rate Q s (Pa ⁇ m 3 / s) represented by (1) using the state equation of gas, the following formula (2), the flow rate Q s' (mol represented by (3) / s), the flow rate Q s '' (g / s) in a possible unit conversion, where the flow rate Q s of the following formula (3) 'was determined' (g / s).
  • the flow rate can be obtained independently for each gas type according to the equations (1) to (3).
  • P R was calculated by multiplying the composition of the mixed gas pressure minus the zero point from the measured values of the pressure measurement section 30, the conductance portion 28 upstream of the calibrated gas species the partial pressure, M As the molecular weight of the gas species to be calibrated.
  • the flow rate Q s ′′ (g / s) of the measurement gas flowing out from the conductance unit 28 obtained by the equation (3) is set as the flow rate of the measurement gas flowing out into the vacuum unit 41, and this flow rate (g Calibration curve for the calibration from the correlation between the ionization vacuum gauge (Pa) and the quadrupole mass spectrometer (A) as the gas permeability measuring unit 43 and the measured value obtained by subtracting the zero point. obtain.
  • FIG. 2 shows a calibration curve graph in the example.
  • the gas barrier film 2 was a high barrier film (sample diameter: ⁇ 50 mm, transmission part diameter: ⁇ 40 mm) mainly composed of polyethylene naphthalate (PEN).
  • the vacuum pumps 17 and 42 are operated to evacuate the gas permeability measuring device 1.
  • the on-off valve 26 of the measurement channel 25 is opened, and the on-off valve 23 of the gas supply unit 21 is opened in a state where the on-off valve 29 of the calibration channel 27 is closed.
  • Supply of water vapor is started.
  • the exposure conditions for water vapor are 1 atmosphere, 40 ° C., and 90% humidity.
  • the measurement gas flows into the gas exposure chamber A from the gas exposure side holding unit 11 side via the measurement flow path 25, and part of the gas passes through the gas barrier film 2 and flows out into the gas transmission chamber B. As a result, it flows out to the vacuum part 41 from the measurement gas permeation side holding part 13 side. Waiting for the measurement value of the gas permeability measuring unit 43 to become constant, information on the flow rate of the measurement gas flowing into the vacuum unit 41 is measured.
  • the calibration gas for calibration is used to quantify the flow rate of the measurement gas that has permeated the gas barrier film 2, and thereby the gas permeability of the gas barrier film 2 is determined.
  • the amount of the measurement gas transmitted is extremely small, and a slight gas release generated in the apparatus is Since the influence is increased, a sample material such as a stainless steel plate that can ignore the amount of the measurement gas permeated is held in the film holding chamber 10 instead of the gas barrier film 2, and the gas permeability measurement unit 43 performs measurement at that time.
  • the gas permeability of the gas barrier film 2 can be determined more accurately.
  • a stainless steel plate is used as the sample, and the difference ( ⁇ P) between the measured values of the gas barrier film 2 of the ionization vacuum gauge as the gas permeability measuring unit 43 and the sample is taken, and the gas permeability of the gas barrier film 2 is taken. It was decided to decide.
  • FIG. 3 the measurement graph regarding the gas permeability in an Example is shown. Incidentally, in FIG.
  • [Delta] P is 1.04 ⁇ 10 -6 Pa
  • the gas permeation amount obtained from the calibration curve for the calibration corresponding to the [Delta] P water vapor transmission amount
  • 8.06 ⁇ 10 - 6 g / day
  • the gas permeability water vapor permeability
  • the gas permeability measuring device of the present invention can simplify the calibration work without removing the gas permeability measuring unit and can accurately measure the gas permeability. It can be widely used for measurement of gas permeability of gas barrier films having various characteristics.

Abstract

[Problem] To simplify a calibration operation and to accurately measure gas permeability. [Solution] A gas permeability measuring device (1) has: a film holding chamber (10) that is capable of holding a gas barrier film (2) between a gas-exposure-side holding part (11) that is arranged on a gas exposure surface side and a gas-transmission-side holding part (13) that is arranged on a gas transmission surface side; a gas upstream part (20) that is provided with an openable and closable measurement flow channel (25), and with a calibration flow channel (27) that is openable and closable so as to be open when the measurement flow channel (25) is closed and that has a calibration measurement part that can measure the flow rate of a measurement gas when the calibration flow channel (27) is open; and a gas downstream part (40) that is provided with a vacuum part (41) that is connected to the gas-transmission-side holding part (13), with a vacuum pump (42), and with a gas permeability measuring part (43) that, when calibrated, is capable of measuring the flow rate of the measurement gas when the gas barrier film (2) is not being held and the flow rate of the measurement gas that is transmitted when the gas barrier film (2) is being held.

Description

ガス透過度測定装置Gas permeability measuring device
　本発明は、ガスバリアフィルムのガス透過度を測定する測定部と、該測定部の校正を行う校正部とを有するガス透過度測定装置に関する。 The present invention relates to a gas permeability measuring apparatus having a measuring unit for measuring the gas permeability of a gas barrier film and a calibration unit for calibrating the measuring unit.
　ガスバリアフィルムは、食品、薬品、電子部品等の包装分野及び電子部品の封止分野等の種々の分野において、重要な役割を果たすことが期待されている。前記ガスバリアフィルムは、そのガスバリア特性、即ち、ガス透過度に応じて使用されることとなるため、前記ガスバリアフィルムの前記ガス透過度の正確な測定は、前記役割を果たす上で、極めて重要な事項となる。 Gas barrier films are expected to play an important role in various fields such as the packaging field for food, medicine, electronic parts, etc., and the sealing field for electronic parts. Since the gas barrier film is used according to its gas barrier properties, that is, gas permeability, the accurate measurement of the gas permeability of the gas barrier film is extremely important for the role. It becomes.
　前記ガスバリアフィルムの前記ガス透過度を測定する装置としては、例えば、フィルムを保持するためのフランジと、前記フィルムにガスを暴露するための容器と、前記フィルムのガス暴露面と逆側のガス透過面に対して所定の圧力まで排気することが可能な真空部とが接続され、前記真空部に取付けられる質量分析計により、前記ガス透過面から前記真空部内に透過するガスのガス透過度を測定する装置が提案されている（特許文献１参照）。 As an apparatus for measuring the gas permeability of the gas barrier film, for example, a flange for holding the film, a container for exposing the gas to the film, and a gas permeation on the opposite side of the gas exposure surface of the film A vacuum unit capable of exhausting to a predetermined pressure with respect to the surface is connected, and the gas permeability of the gas permeating from the gas transmission surface into the vacuum unit is measured by a mass spectrometer attached to the vacuum unit An apparatus has been proposed (see Patent Document 1).
　しかしながら、前記装置では、前記質量分析計を校正する手段を有しないため、前記質量分析計を校正するためには、前記装置から前記質量分析計を取外し、適当な校正手段を用いて校正する必要がある。この場合、校正作業が煩雑化するだけでなく、取外し・輸送・取付け作業に伴う再現性や、校正時と測定時における環境条件（温度等）及び設置向きの違いによって、前記質量分析計の感度特性が変化してしまい、ガス透過度の正確な測定ができなくなる場合がある。
また、前記質量分析計が取付けられる校正用のガス流路系と、前記装置のガス流路系とが異なるため、前記校正用のガス流路系で校正された前記質量分析計を用いて前記装置のガス流路系における前記ガス透過度を測定した場合、前記校正が前記装置のガス流路系における前記ガスの流量を反映できず、前記ガスバリアフィルムの前記ガス透過度を正確に測定できない問題がある。 However, since the apparatus does not have means for calibrating the mass spectrometer, in order to calibrate the mass spectrometer, it is necessary to remove the mass spectrometer from the apparatus and calibrate it using an appropriate calibration means. There is. In this case, not only the calibration work becomes complicated, but also the sensitivity of the mass spectrometer depends on the reproducibility associated with the removal / transport / installation work, the environmental conditions (temperature, etc.) during calibration and measurement, and the difference in installation orientation. The characteristics may change, and accurate measurement of gas permeability may not be possible.
Further, since the gas flow path system for calibration to which the mass spectrometer is attached is different from the gas flow path system of the apparatus, the mass spectrometer calibrated with the gas flow path system for calibration is used. When the gas permeability in the gas flow path system of the apparatus is measured, the calibration cannot reflect the flow rate of the gas in the gas flow path system of the apparatus, and the gas permeability of the gas barrier film cannot be accurately measured There is.
　更に、ガスバリアフィルムの実使用条件に近い湿潤環境、例えば、水蒸気と酸素の混合ガスを用いたガス雰囲気での適切なガスバリア性の評価手法の開発が求められているが、適切な校正・評価方法が存在しないため、実用化されていなのが現状である。 Furthermore, there is a need for the development of an appropriate gas barrier property evaluation method in a humid environment close to the actual use conditions of the gas barrier film, for example, a gas atmosphere using a mixed gas of water vapor and oxygen. Is not in practical use because there is no existing.
特開平６－２４１９７８号公報Japanese Patent Laid-Open No. 6-241978
　本発明は、従来における前記諸問題を解決し、以下の目的を達成することを課題とする。即ち、本発明は、ガス透過度測定部を取外すことなく、その校正作業を簡素化可能とするとともに、正確にガス透過度を測定可能なガス透過度測定装置を提供することを目的とする。 This invention makes it a subject to solve the said various problems in the past and to achieve the following objectives. That is, an object of the present invention is to provide a gas permeability measuring apparatus capable of simplifying the calibration operation without removing the gas permeability measuring unit and accurately measuring the gas permeability.
　前記課題を解決するための手段としては、以下の通りである。即ち、
　＜１＞　ガスバリアフィルムのガス暴露面側に配されるガス暴露側保持部と前記ガスバリアフィルムのガス透過面側に配されるガス透過側保持部とで前記ガスバリアフィルムの周部を挟持して保持可能とされ、前記ガスバリアフィルムを保持させたときに、測定用ガスが流入される前記ガス暴露面と前記ガス暴露側保持部とで画成されるガス暴露室、及び、前記ガス透過面から透過する前記測定用ガスが流入される前記ガス透過面と前記ガス透過側保持部とで画成されるガス透過室が形成されるフィルム保持室と、前記測定用ガスを供給するガス供給部、前記ガス供給部－前記ガス暴露側保持部間に配される開閉自在の測定用流路、及び、前記ガス供給部－前記ガス暴露側保持部間に配され、前記測定用流路を閉状態としたとき開状態とされ、前記測定用流路を開状態としたとき閉状態とされるように開閉自在とされ、開状態において前記ガスバリアフィルムを保持しない状態の前記フィルム保持室に流入させる前記測定用ガスの流量を測定可能な校正用測定部を有する校正用流路を備えるガス上流部と、前記ガス透過側保持部と接続される中空の真空部、前記真空部内を排気する真空ポンプ、及び、前記真空部に取付けられ、前記ガスバリアフィルムを保持しない状態の前記フィルム保持室から流出する前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされるとともに、前記ガスバリアフィルムを保持した状態で前記ガス透過室から流出する前記ガスバリアフィルムを透過した前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされるガス透過度測定部を備えるガス下流部と、を有することを特徴とするガス透過度測定装置。
　＜２＞　フィルム保持室に流入される測定用ガスの流入方向に沿ってガス透過側保持部から前記測定用ガスを流出させるとともに、真空部が前記流入方向に沿って中空とされ、前記流入方向の延長位置に真空ポンプが配されるように構成される前記＜１＞に記載のガス透過度測定装置。
　＜３＞　校正用測定部が、オリフィス、細管及び多孔質体の少なくともいずれかで形成され、コンダクタンスが予め測定されたコンダクタンス部と、前記コンダクタンス部に流入される測定用ガスの圧力を測定する圧力測定部と、を有する前記＜１＞から＜２＞のいずれかに記載のガス透過度測定装置。
　＜４＞　コンダクタンス部が、分子流条件を満たす状態で測定用ガスを流通可能とされる前記＜３＞に記載のガス透過度測定装置。 Means for solving the problems are as follows. That is,
<1> The gas barrier film holding portion disposed on the gas exposure surface side of the gas barrier film and the gas permeation side holding portion disposed on the gas permeation surface side of the gas barrier film sandwich and hold the peripheral portion of the gas barrier film. When the gas barrier film is held, the gas exposure chamber defined by the gas exposure surface into which the measurement gas flows and the gas exposure side holding portion, and the gas transmission surface transmit the gas barrier film. A film holding chamber in which a gas permeation chamber defined by the gas permeation surface into which the measurement gas is introduced and the gas permeation side holding portion is formed, a gas supply portion for supplying the measurement gas, An openable and closable measurement channel disposed between a gas supply unit and the gas exposure side holding unit, and a measurement channel disposed between the gas supply unit and the gas exposure side holding unit, wherein the measurement channel is closed. When opened, It can be opened and closed so that it is closed when the measurement channel is in the open state, and the flow rate of the measurement gas flowing into the film holding chamber in the state where the gas barrier film is not held in the open state can be measured. A gas upstream portion having a calibration flow path having a calibration measuring portion, a hollow vacuum portion connected to the gas permeation side holding portion, a vacuum pump for exhausting the inside of the vacuum portion, and attached to the vacuum portion The flow rate of the measurement gas flowing out from the film holding chamber in a state where the gas barrier film is not held can be calibrated and measured by the calibration measuring unit, and the gas permeation can be performed while the gas barrier film is held. Gas permeation that can be measured by calibrating the flow rate of the measurement gas that has passed through the gas barrier film flowing out of the chamber by the calibration measurement unit Gas permeability measurement apparatus and having a gas downstream portion comprising a measuring unit.
<2> The measurement gas is caused to flow out from the gas permeation-side holding portion along the inflow direction of the measurement gas flowing into the film holding chamber, and the vacuum portion is hollow along the inflow direction. The gas permeability measuring device according to <1>, wherein a vacuum pump is disposed at an extended position of the gas pump.
<3> A calibration measurement unit is formed of at least one of an orifice, a thin tube, and a porous body, and a conductance unit whose conductance is measured in advance, and a pressure for measuring the pressure of the measurement gas flowing into the conductance unit The gas permeability measuring device according to any one of <1> to <2>, further including a measuring unit.
<4> The gas permeability measuring device according to <3>, wherein the conductance part can flow the measurement gas in a state where the molecular flow condition is satisfied.
　本発明によれば、従来技術における前記諸問題を解決することができ、ガス透過度測定部を取外すことなく、その校正作業を簡素化可能とするとともに、正確にガス透過度を測定可能なガス透過度測定装置を提供することができる。 According to the present invention, the above-mentioned problems in the prior art can be solved, and the calibration operation can be simplified and the gas permeability can be accurately measured without removing the gas permeability measuring unit. A transmittance measuring device can be provided.
校正時のガス透過度測定装置の概要を示す説明図である。It is explanatory drawing which shows the outline | summary of the gas permeability measuring apparatus at the time of calibration. 測定時のガス透過度測定装置の概要を示す説明図である。It is explanatory drawing which shows the outline | summary of the gas permeability measuring apparatus at the time of a measurement. 実施例における検量線グラフを示す図である。It is a figure which shows the calibration curve graph in an Example. 実施例におけるガス透過度に関する測定グラフを示す図である。It is a figure which shows the measurement graph regarding the gas permeability in an Example.
　本発明のガス透過度測定装置の一実施形態を図１（ａ），（ｂ）を参照しつつ、説明する。図１（ａ）は、校正時のガス透過度測定装置の概要を示す説明図であり、図１（ｂ）は、測定時のガス透過度測定装置の概要を示す説明図である。
　図１（ａ），（ｂ）に示すように、ガス透過度測定装置１は、フィルム保持室１０と、ガス上流部２０と、ガス下流部４０とを有する。 An embodiment of the gas permeability measuring apparatus of the present invention will be described with reference to FIGS. 1 (a) and 1 (b). Fig.1 (a) is explanatory drawing which shows the outline | summary of the gas permeability measuring apparatus at the time of calibration, and FIG.1 (b) is explanatory drawing which shows the outline | summary of the gas permeability measuring apparatus at the time of measurement.
As shown in FIGS. 1A and 1B, the gas permeability measuring device 1 includes a film holding chamber 10, a gas upstream portion 20, and a gas downstream portion 40.
　フィルム保持室１０は、ガスバリアフィルム２のガス暴露面側に配されるガス暴露側保持部１１と、ガスバリアフィルム２のガス暴露面と反対側のガス透過面側に配されるガス透過側保持部１３とを有する。これらガス暴露側保持部１１とガス透過側保持部１３とは、ガスバリアフィルム２を介して対向配置され、ガスバリアフィルム２の周部を挟持して保持可能とされる。
　ガスバリアフィルム２を保持させたとき（図１（ｂ）参照）、測定用ガスが流入される前記ガス暴露面とガス暴露側保持部１１とで画成されるガス暴露室Ａと、前記ガス透過面から透過する前記測定用ガスが流入される前記ガス透過面とガス透過側保持部１３とで画成されるガス透過室Ｂが形成される。
　ガス暴露側保持部１１とガス透過側保持部１３とは、ガス暴露室Ａ及びガス透過室Ｂにおいて、ガスバリアフィルム２が十分な量の前記測定用ガスに暴露され、その透過量を測定できる大きさを有する。
　また、ガス暴露側保持部１１とガス透過側保持部１３とは、ガス暴露室Ａ及びガス透過室Ｂの気密性を保持するため、Ｏリング等のシール部材１２，１４を有し、シール部材１２，１４の間にガスバリアフィルム２の周部を挟持させて、これを保持する。 The film holding chamber 10 includes a gas exposure side holding portion 11 disposed on the gas exposure surface side of the gas barrier film 2 and a gas permeation side holding portion disposed on the gas transmission surface side opposite to the gas exposure surface of the gas barrier film 2. 13. The gas exposure side holding part 11 and the gas permeation side holding part 13 are arranged to face each other with the gas barrier film 2 interposed therebetween, and can be held by holding the peripheral part of the gas barrier film 2.
When the gas barrier film 2 is held (see FIG. 1B), the gas exposure chamber A defined by the gas exposure surface into which the measurement gas flows and the gas exposure side holding unit 11 are formed, and the gas permeation A gas permeation chamber B defined by the gas permeation surface into which the measurement gas permeating from the surface flows and the gas permeation side holding portion 13 is formed.
The gas exposure side holding part 11 and the gas permeation side holding part 13 are large enough that the gas barrier film 2 is exposed to a sufficient amount of the measuring gas in the gas exposure chamber A and the gas permeation chamber B, and the permeation amount can be measured. Have
Further, the gas exposure side holding part 11 and the gas permeation side holding part 13 have seal members 12, 14 such as O-rings in order to maintain the gas tightness of the gas exposure chamber A and the gas permeation chamber B. The peripheral part of the gas barrier film 2 is sandwiched between 12 and 14 and held.
　フィルム保持室１０としては、シール部材１２，１４の間からガス暴露室Ａ及びガス透過室Ｂに侵入するリークガスを排除するため、これらシール部材１２，１４の外方を覆い、排気室Ｃを形成する排気部１５を有していてもよい。この場合、排気室Ｃ内のガスは、開閉弁１６を開いた状態で、真空ポンプ１７を作動させて排気される。
　なお、ガスバリアフィルム２を保持しない状態（図１（ａ））では、フィルム保持室１０は、ガス暴露側保持部１１とガス透過側保持部１３とで画成される気密性の空間を形成可能とされる。 The film holding chamber 10 covers the outside of the seal members 12 and 14 and forms an exhaust chamber C in order to eliminate leak gas that enters the gas exposure chamber A and the gas permeation chamber B from between the seal members 12 and 14. You may have the exhaust part 15 to do. In this case, the gas in the exhaust chamber C is exhausted by operating the vacuum pump 17 with the on-off valve 16 open.
In the state where the gas barrier film 2 is not held (FIG. 1A), the film holding chamber 10 can form an airtight space defined by the gas exposure side holding part 11 and the gas permeation side holding part 13. It is said.
　ガス上流部２０は、前記測定用ガスを供給するガス供給部２１，２２と、ガス供給部２１，２２とガス暴露側保持部１１との間に配される開閉自在の測定用流路２５と、同じくガス供給部２１，２２とガス暴露側保持部１１との間に配される校正用流路２７とで構成される。 The gas upstream section 20 includes gas supply sections 21 and 22 that supply the measurement gas, and an openable and closable measurement flow path 25 that is disposed between the gas supply sections 21 and 22 and the gas exposure side holding section 11. Similarly, the calibration flow path 27 is arranged between the gas supply units 21 and 22 and the gas exposure side holding unit 11.
　ガス供給部２１，２２は、開閉弁２３，２４を開いた状態で、測定用流路２５又は校正用流路２７に前記測定用ガスを供給する。ガス供給部２１，２２としては、いずれか１つであってもよく、３つ以上有していてもよい。２種以上の混合ガスを用いてガスバリアフィルム２のガス透過度を測定する場合や２種以上の純ガスを順番に供給してガスバリアフィルム２のそれぞれのガス透過度を測定する場合には、２つ以上とする。
　なお、前記測定用ガスとしては、ガスバリアフィルム２に対するガス透過度測定の目的に応じて適宜選択することができる。 The gas supply units 21 and 22 supply the measurement gas to the measurement flow path 25 or the calibration flow path 27 with the on-off valves 23 and 24 being opened. As gas supply parts 21 and 22, any one may be sufficient and you may have three or more. When measuring the gas permeability of the gas barrier film 2 using two or more kinds of mixed gases, or when measuring the gas permeability of each of the gas barrier films 2 by sequentially supplying two or more kinds of pure gases, 2 More than one.
The measurement gas can be appropriately selected according to the purpose of measuring the gas permeability with respect to the gas barrier film 2.
　測定用流路２５は、流路中に開閉弁２６を有し、ガス供給部２１，２２から供給される前記測定用ガスをガス暴露側保持部１１に移送する。また、校正用流路２７は、流路中に開閉弁２９を有し、ガス供給部２１，２２から供給される前記測定用ガスをガス暴露側保持部１１に移送する。
　校正用流路２７は、フィルム保持室１０がガスバリアフィルム２を保持しない状態（図１（ａ））において用いられ、測定用流路２５を閉状態としたとき開状態とされる。また、測定用流路２５は、フィルム保持室１０がガスバリアフィルム２を保持する状態（図１（ｂ））において用いられ、測定用流路２５を開状態としたときは、校正用流路２７を閉状態とする。
　即ち、ガスバリアフィルム２を保持しない状態とガスバリアフィルム２を保持する状態とで、いずれか一方の流路が開状態とされ、ガス供給部２１，２２から供給される前記測定用ガスをガス暴露側保持部１１に移送する。
　なお、図示しないが、一端側が測定用流路２５及び校正用流路２７と接続され、ガス透過度の測定前に測定用流路２５及び校正用流路２７内を排気する排気流路を配してもよい。この場合、例えば、前記排気用流路の他端側を真空ポンプ１７に接続し、測定用流路２５及び校正用流路２７内を排気するように構成することができる。 The measurement channel 25 has an open / close valve 26 in the channel, and transfers the measurement gas supplied from the gas supply units 21 and 22 to the gas exposure side holding unit 11. The calibration flow path 27 has an open / close valve 29 in the flow path, and transfers the measurement gas supplied from the gas supply units 21 and 22 to the gas exposure side holding unit 11.
The calibration flow path 27 is used when the film holding chamber 10 does not hold the gas barrier film 2 (FIG. 1A), and is opened when the measurement flow path 25 is closed. The measurement channel 25 is used in a state where the film holding chamber 10 holds the gas barrier film 2 (FIG. 1B). When the measurement channel 25 is opened, the calibration channel 27 is used. Is closed.
That is, one of the flow paths is opened in a state where the gas barrier film 2 is not held and a state where the gas barrier film 2 is held, and the measurement gas supplied from the gas supply units 21 and 22 is supplied to the gas exposure side. Transfer to the holding unit 11.
Although not shown, one end side is connected to the measurement flow path 25 and the calibration flow path 27, and an exhaust flow path for exhausting the measurement flow path 25 and the calibration flow path 27 is arranged before measuring the gas permeability. May be. In this case, for example, the other end side of the exhaust passage can be connected to the vacuum pump 17 so that the inside of the measurement passage 25 and the calibration passage 27 can be exhausted.
　校正用流路２７は、開状態において、ガスバリアフィルム２を保持しない状態のフィルム保持室１０に流入させる前記測定用ガスの流量を測定する校正用測定部を有する。
　前記校正用測定部の具体的な構成としては、特に制限はないが、前記測定用ガスの流用を正確に測定する観点から、オリフィス、細管及び多孔質体の少なくともいずれかで構成され、流通するガスのコンダクタンスが予め測定されたコンダクタンス部２８と、前記コンダクタンス部２８に流入される前記測定用ガスの圧力を測定する圧力測定部３０とで構成されることが好ましい。なお、コンダクタンス部２８としては、オリフィス、細管及び多孔質体を組み合わせて構成してもよい。前記測定用ガスとして前記混合ガスを用いる場合には、多孔質体として、特開２０１１－４７８５５号公報に記載の微小孔フィルタを好適に用いることができる。また、圧力測定部３０としては、公知の圧力計等を用いることができるが、気体の種類によって特性が変化しない圧力計（隔膜真空計など）を用いることが好ましい。また、水蒸気のガス透過度試験を行う場合、湿度計を設置する場合もある。 The calibration flow path 27 has a calibration measurement unit that measures the flow rate of the measurement gas that flows into the film holding chamber 10 in the open state without holding the gas barrier film 2.
The specific configuration of the calibration measuring unit is not particularly limited, but from the viewpoint of accurately measuring the diversion of the measuring gas, the calibration measuring unit is configured by at least one of an orifice, a thin tube, and a porous body and circulates. It is preferable to include a conductance unit 28 in which the gas conductance is measured in advance, and a pressure measurement unit 30 that measures the pressure of the measurement gas flowing into the conductance unit 28. The conductance portion 28 may be configured by combining an orifice, a thin tube, and a porous body. When the mixed gas is used as the measurement gas, a microporous filter described in JP 2011-47855 A can be suitably used as the porous body. As the pressure measuring unit 30, a known pressure gauge or the like can be used, but a pressure gauge (such as a diaphragm vacuum gauge) whose characteristics do not change depending on the type of gas is preferably used. In addition, when performing a water vapor gas permeability test, a hygrometer may be installed.
　また、前記測定用ガスとして前記混合ガスを用いる場合、コンダクタンス部２８が分子流条件を満たす状態で前記測定用ガスを流通可能とされることが好ましい。前記分子流条件を満たすと、気体の種類によるコンダクタンスの違いを分子量だけで補正できると共に、前記混合ガス中の各ガス種の相互作用を排除することができるので、コンダクタンス部２８に供給される前記混合ガスの組成比及び圧力から、コンダクタンス部２８から流出する前記混合ガスの流量、流量比を求めることができる。なお、前記分子量条件を満たすためには、前記コンダクタンス部２８に供給される前記混合ガスの圧力が所定の範囲となるように制御可能であることが必要とされる。
　このようにガス透過度測定装置１では、純ガス、混合ガスのガス構成及びガス種を問わず、ガス透過度測定部４３を（取外すことなく）校正することが可能で、得られた校正結果に基づき、これらで構成される前記測定用ガスのガスバリアフィルム２に対するガス透過度を正確に測定することができる。 When the mixed gas is used as the measurement gas, it is preferable that the measurement gas can be circulated in a state where the conductance part 28 satisfies the molecular flow condition. When the molecular flow condition is satisfied, the difference in conductance due to the type of gas can be corrected only by the molecular weight, and the interaction of each gas type in the mixed gas can be eliminated. From the composition ratio and pressure of the mixed gas, the flow rate and flow rate ratio of the mixed gas flowing out from the conductance unit 28 can be obtained. In order to satisfy the molecular weight condition, it is necessary that the pressure of the mixed gas supplied to the conductance unit 28 can be controlled within a predetermined range.
Thus, in the gas permeability measuring apparatus 1, it is possible to calibrate (without removing) the gas permeability measuring unit 43 regardless of the gas configuration and gas type of pure gas or mixed gas, and the obtained calibration result On the basis of the above, the gas permeability of the measuring gas composed of these to the gas barrier film 2 can be accurately measured.
　ガス下流部４０は、ガス透過側保持部１３と接続される中空の真空部４１と、真空部４１内を排気する真空ポンプ４２と、真空部４１に取付けられるガス透過度測定部４３とで構成される。 The gas downstream portion 40 includes a hollow vacuum portion 41 connected to the gas permeation side holding portion 13, a vacuum pump 42 that exhausts the inside of the vacuum portion 41, and a gas permeability measurement portion 43 attached to the vacuum portion 41. Is done.
　真空部４１としては、公知の真空容器により構成することができ、ハイバリア性のフィルムに対する測定を考慮して、１０－４Ｐａ以下の圧力に排気できることが好ましい。また、真空ポンプ４２としては、真空ポンプ１７も同様に、拡散ポンプ、ターボ分子ポンプ、クライオポンプ、スパッタイオンポンプ、ゲッターポンプ等の公知のポンプを用いることができる。なお、真空ポンプ４２としては、真空部４１内の圧力を低く保持するために、高真空、超高真空用途のものが好ましい。 The vacuum part 41 can be constituted by a known vacuum container, and it is preferable that the pressure can be evacuated to 10 −4 Pa or less in consideration of measurement with respect to a high barrier film. Similarly, as the vacuum pump 42, a known pump such as a diffusion pump, a turbo molecular pump, a cryopump, a sputter ion pump, and a getter pump can be used as the vacuum pump 17. The vacuum pump 42 is preferably used for high vacuum or ultra-high vacuum in order to keep the pressure in the vacuum part 41 low.
　ガス透過度測定部４３は、ガスバリアフィルム２を保持しない状態（図１（ａ））のフィルム保持室１０から流出する前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされるとともに、ガスバリアフィルム２を保持した状態（図１（ｂ））でガス透過室Ｂから流出するガスバリアフィルム２を透過した前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされる。
　こうしたガス透過度測定部４３としては、電離真空計等の公知の真空計、四重極質量分析計等の公知の質量分析計を用いることができる。 The gas permeability measurement unit 43 can measure the flow rate of the measurement gas flowing out from the film holding chamber 10 in a state where the gas barrier film 2 is not held (FIG. 1A) by the calibration measurement unit. In addition, the flow rate of the measurement gas that has permeated the gas barrier film 2 flowing out from the gas permeation chamber B in a state where the gas barrier film 2 is held (FIG. 1B) can be calibrated and measured by the calibration measurement unit. Is done.
As the gas permeability measuring unit 43, a known vacuum gauge such as an ionization vacuum gauge or a known mass spectrometer such as a quadrupole mass spectrometer can be used.
　ガス透過度測定装置１では、フィルム保持室１０に流入される前記測定用ガスの流入方向に沿ってガス透過側保持部１３から前記測定用ガスを流出させるように構成され、真空部４１が前記流入方向に沿って中空とされ、真空ポンプ４２が前記流入方向の延長位置に配されるように構成される。このように構成されることで、フィルム保持室１０に流入される前記測定用ガスが部分的な偏りを有することなく、ガス透過側保持部１３から流出されるとともに、流出した前記測定用ガスが真空部４１内で部分的な偏りを有することを排除することができ、挙動が安定した前記測定用ガスの流量をガス透過度測定部４３で測定可能とされる。 The gas permeability measuring apparatus 1 is configured to cause the measurement gas to flow out from the gas permeation-side holding unit 13 along the inflow direction of the measurement gas flowing into the film holding chamber 10, and the vacuum unit 41 includes the vacuum unit 41. It is hollow along the inflow direction, and the vacuum pump 42 is arranged at an extended position in the inflow direction. By being configured in this way, the measurement gas flowing into the film holding chamber 10 flows out from the gas permeation-side holding unit 13 without partial deviation, and the outflowed measurement gas flows. It is possible to eliminate partial deviation in the vacuum part 41, and the gas permeability measuring part 43 can measure the flow rate of the measuring gas with a stable behavior.
　以上に説明したガス透過度測定装置１では、ガスバリアフィルム２を保持しない状態（図１（ａ））で、ガス供給部２１，２２から供給される前記測定用ガスを校正用流路２７を介してフィルム保持室１０に流入させ、その流量をガス透過度測定部４３で測定可能とされる。即ち、校正用流路２７中の前記校正用測定部を構成するコンダクタンス部２８から流出する前記測定用ガスの流量を、圧力測定部３０で測定した圧力、コンダクタンス部２８のコンダクタンス及び温度から算出し、この流量とガス透過度測定部４３の指示値を相関させて、フィルム保持室１０、延いては真空部４１に流入する前記測定用ガスの流量に対応するガス透過度測定部４３の指示値の検量線が作成可能とされる。 In the gas permeability measuring apparatus 1 described above, the measurement gas supplied from the gas supply units 21 and 22 is passed through the calibration channel 27 without holding the gas barrier film 2 (FIG. 1A). Then, the gas is allowed to flow into the film holding chamber 10, and the flow rate thereof can be measured by the gas permeability measuring unit 43. That is, the flow rate of the measurement gas flowing out from the conductance unit 28 constituting the calibration measurement unit in the calibration channel 27 is calculated from the pressure measured by the pressure measurement unit 30, the conductance and temperature of the conductance unit 28. By correlating the flow rate with the indicated value of the gas permeability measuring unit 43, the indicated value of the gas permeability measuring unit 43 corresponding to the flow rate of the measuring gas flowing into the film holding chamber 10, and then the vacuum part 41, is obtained. A calibration curve can be created.
　ガスバリアフィルム２を保持した状態（図１（ｂ））では、ガス供給部２１，２２から供給される前記測定用ガスを測定用流路２５を介してフィルム保持室１０のガス暴露室Ａに流入させ、ガスバリアフィルム２を透過しガス透過室Ｂから流出する前記測定用ガス（透過ガス）の流量をガス透過度測定部４３で測定可能とされる。即ち、ガスバリアフィルム２を保持しない状態（図１（ａ））で得られた前記検量線に基づき、ガス透過度測定部４３の指示値に対応する前記測定用ガス（透過ガス）の流量を求めることができる。 In the state where the gas barrier film 2 is held (FIG. 1B), the measurement gas supplied from the gas supply units 21 and 22 flows into the gas exposure chamber A of the film holding chamber 10 through the measurement channel 25. The gas permeability measuring unit 43 can measure the flow rate of the measurement gas (permeated gas) that passes through the gas barrier film 2 and flows out of the gas permeation chamber B. That is, based on the calibration curve obtained without holding the gas barrier film 2 (FIG. 1A), the flow rate of the measuring gas (permeating gas) corresponding to the indicated value of the gas permeability measuring unit 43 is obtained. be able to.
　このように構成されるガス透過度測定装置１では、装置内にガス透過度測定部４３を校正するための前記校正用測定部を有する校正用流路２７が配されるため、いちいちガス透過度測定装置４３を装置から取外して校正し、校正後、装置に取付ける作業を省くことができ、校正作業を簡素化することができる。
　また、ガス上流部２０に前記校正用測定部を有する校正用流路２７を配することで、校正用流路２７及び測定用流路２５からフィルム保持室１０に流入する前記測定用ガスのガス透過度測定部４３に至る流通経路を同一とする（図１（ａ），（ｂ）中のガス流通経路を示す矢印を参照）ことから、校正時におけるガス透過度測定部４３の前記測定用ガスの測定条件を測定時のものと共通させることができ、校正時のガス透過度測定部４３の指示値に高い信頼性が確保される。したがって、ガス透過度測定装置１では、測定時において、校正時に作成される信頼性の高い検量線に基づき、正確なガス透過度を測定することができる。
　ここで、装置内に校正部を設ける場合、測定用流路２５のみをガス上流部２０に配し、校正用流路２７をガス下流部４０の真空部４１に配する構成も検討されるが、この構成では、フィルム保持室１０に流入される前記測定ガスのガス透過度測定部４３に至る流通経路が、校正時と測定時の場合とで異なるため、両者の間で真空部４１内の圧力分布や飛行する気体分子の方向分布に変化が生じる。したがって、前記測定ガスの流通条件の相違による影響を受け、校正時に作成される検量線に基づき、測定時に測定されるガス透過度の測定結果に対する信頼性を低下させることとなる。
　なお、ガス透過度測定装置１は、本発明の一実施形態を例示したものであり、前述の効果を奏する限り、本発明の技術的思想は、これに限定されるものではない。 In the gas permeability measuring apparatus 1 configured as described above, since the calibration flow path 27 having the calibration measuring section for calibrating the gas permeability measuring section 43 is arranged in the apparatus, the gas permeability is measured one by one. The measuring device 43 can be removed from the device and calibrated. After the calibration, the work of attaching to the device can be omitted, and the calibration work can be simplified.
Further, by providing the calibration flow path 27 having the calibration measurement section in the gas upstream section 20, the gas of the measurement gas flowing into the film holding chamber 10 from the calibration flow path 27 and the measurement flow path 25. Since the flow path to the permeability measuring unit 43 is the same (refer to the arrows indicating the gas flow paths in FIGS. 1A and 1B), the gas permeability measuring unit 43 is used for the measurement at the time of calibration. Gas measurement conditions can be made common with those at the time of measurement, and high reliability is ensured for the indicated value of the gas permeability measurement unit 43 at the time of calibration. Therefore, the gas permeability measuring apparatus 1 can measure an accurate gas permeability at the time of measurement based on a highly reliable calibration curve created at the time of calibration.
Here, when the calibration unit is provided in the apparatus, a configuration in which only the measurement channel 25 is arranged in the gas upstream unit 20 and the calibration channel 27 is arranged in the vacuum unit 41 of the gas downstream unit 40 is also considered. In this configuration, the flow path of the measurement gas that flows into the film holding chamber 10 to the gas permeability measurement unit 43 differs between the calibration time and the measurement time. Changes occur in the pressure distribution and the direction distribution of flying gas molecules. Therefore, under the influence of the difference in the flow conditions of the measurement gas, the reliability of the measurement result of the gas permeability measured at the time of measurement is lowered based on the calibration curve created at the time of calibration.
In addition, the gas permeability measuring apparatus 1 illustrates one embodiment of the present invention, and the technical idea of the present invention is not limited to this as long as the above-described effects are exhibited.
　ガス透過度測定装置１を用いたガス透過度の測定方法を、実際の測定例とともに実施例として説明する。即ち、前述のガス透過度測定装置１（図１（ａ），（ｂ）参照）に準じて構成されたガス透過度測定装置を用いてガス透過度の測定を行った際の測定方法及び測定結果について説明する。なお、以下では、説明の便宜上、ガス透過度測定装置１と同じ符号を用いて測定方法及び測定結果を説明する。 A gas permeability measurement method using the gas permeability measuring apparatus 1 will be described as an example together with an actual measurement example. That is, a measurement method and measurement when gas permeability is measured using a gas permeability measuring device configured in accordance with the gas permeability measuring device 1 described above (see FIGS. 1A and 1B). The results will be described. In the following, for convenience of explanation, the measurement method and the measurement results will be described using the same reference numerals as those of the gas permeability measuring apparatus 1.
　先ず、ガスバリアフィルムを保持させない状態（図１（ａ）参照）で、真空ポンプ１７，４２をそれぞれ作動させ、ガス透過度測定装置１内を真空排気させる。次いで、この状態の圧力測定部３０、ガス透過度測定部４３の計測値をゼロ点として記録する。次いで、測定用流路２５の開閉弁２６を閉め、校正用流路２７の開閉弁２９を開けた状態で、ガス供給部２１の開閉弁２３を開け、ガス供給部２１から測定用ガスの供給を開始する。前記測定用ガスは、校正用流路２７を経由してガス暴露側保持部１１側からフィルム保持室１０に流入し、ガス透過側保持部１３側から真空部４１に流出する。次いで、圧力測定部３０，ガス透過度測定部４３の計測値が一定となるのを待ち、前記測定用ガスのコンダクタンス部２８流入前の圧力を圧力測定部３０で計測するとともに、真空部４１内に流出した前記測定用ガスの流量に関する情報を計測する。
　測定は、前記測定用ガスとして、水蒸気を用い、ガス透過度測定部４３として、電離真空計及び四重極質量分析計を用いて行った。
　なお、圧力測定部３０で計測されるコンダクタンス部２８流入前の圧力は、ガス供給部２１からの前記測定用ガスの供給量を調整することで、コンダクタンス部２８を流通する前記測定用ガスの流れが分子流条件を満たすように制御可能とされる。 First, in a state where the gas barrier film is not held (see FIG. 1A), the vacuum pumps 17 and 42 are operated to evacuate the inside of the gas permeability measuring device 1. Next, the measurement values of the pressure measurement unit 30 and the gas permeability measurement unit 43 in this state are recorded as zero points. Next, with the on-off valve 26 of the measurement channel 25 closed and the on-off valve 29 of the calibration channel 27 opened, the on-off valve 23 of the gas supply unit 21 is opened to supply the measurement gas from the gas supply unit 21. To start. The measurement gas flows into the film holding chamber 10 from the gas exposure side holding unit 11 side through the calibration channel 27 and flows out from the gas permeation side holding unit 13 side to the vacuum unit 41. Next, the pressure measurement unit 30 and the gas permeability measurement unit 43 wait for the measurement values to become constant, and the pressure measurement unit 30 measures the pressure before the conductance unit 28 flows into the measurement gas. Information on the flow rate of the measurement gas that has flowed out is measured.
The measurement was performed using water vapor as the measurement gas, and using an ionization vacuum gauge and a quadrupole mass spectrometer as the gas permeability measurement unit 43.
In addition, the pressure before the conductance part 28 inflow measured by the pressure measurement part 30 adjusts the supply amount of the measurement gas from the gas supply part 21, and thereby the flow of the measurement gas flowing through the conductance part 28 Can be controlled to satisfy the molecular flow condition.
　こうした条件において、コンダクタンス部２８を流通し、フィルム保持室１０を経由して、真空部４１に流出する前記測定用ガスの流量Ｑｓ（Ｐａ・ｍ３／ｓ）は、下記式（１）で表される。 Under such conditions, the flow rate Q s (Pa · m 3 / s) of the measurement gas flowing through the conductance part 28 and flowing out to the vacuum part 41 via the film holding chamber 10 is expressed by the following formula (1). expressed.
Figure JPOXMLDOC01-appb-M000001
 　なお、前記式（１）中、ＰＲは、圧力測定部３０の計測値からゼロ点を引いた圧力を示し、Ｃｓは、予め測定しておいたコンダクタンス部２８の代表的な気体（ここでは、窒素ガス）における分子流コンダクタンスを示し、ＭＮ２は、窒素の分子量を示し、Ｍは、前記測定用ガス（水蒸気）の分子量を示し、Ｔ０は、Ｃｓ測定時の温度を示し、Ｔは、前記測定用ガス供給時のガス供給部２１の温度を示す。
　また、前記式（１）で表される流量Ｑｓ（Ｐａ・ｍ３／ｓ）は、気体の状態方程式を用い、下記式（２），（３）で表される流量Ｑｓ’（ｍｏｌ／ｓ）、流量Ｑｓ’’（ｇ／ｓ）に単位変換可能であり、ここでは、下記式（３）で表される流量Ｑｓ’’（ｇ／ｓ）を求めた。
Figure JPOXMLDOC01-appb-M000001
 Incidentally, the formula (1), P R represents the pressure minus the zero point from the measured values of the pressure measuring unit 30, C s is the conductance portion 28 measured in advance typical gas (here in, a molecular flow conductance in nitrogen gas), M N2 represents the molecular weight of nitrogen, M represents a molecular weight of the measuring gas (water vapor), T 0 represents the temperature at C s measurement, T indicates the temperature of the gas supply unit 21 when the measurement gas is supplied.
Further, the flow rate Q s (Pa · m 3 / s) represented by (1), using the state equation of gas, the following formula (2), the flow rate Q s' (mol represented by (3) / s), the flow rate Q s '' (g / s) in a possible unit conversion, where the flow rate Q s of the following formula (3) 'was determined' (g / s).
Figure JPOXMLDOC01-appb-M000002
 　なお、前記測定用ガスとして混合ガスを用いる場合、コンダクタンス部２８が分子流条件を満たすものであれば、前記式（１）～（３）により、ガス種ごとに独立して流量を求めることができ、この場合、ＰＲとして、圧力測定部３０の計測値からゼロ点を引いた圧力に混合ガスの組成を乗じることで求めた、コンダクタンス部２８上流の校正対象のガス種の分圧、Ｍとして校正対象のガス種の分子量を用いる。
Figure JPOXMLDOC01-appb-M000002
 When a mixed gas is used as the measurement gas, if the conductance part 28 satisfies the molecular flow condition, the flow rate can be obtained independently for each gas type according to the equations (1) to (3). can, in this case, as P R, was calculated by multiplying the composition of the mixed gas pressure minus the zero point from the measured values of the pressure measurement section 30, the conductance portion 28 upstream of the calibrated gas species the partial pressure, M As the molecular weight of the gas species to be calibrated.
　前記式（３）で求めたコンダクタンス部２８から流出する前記測定用ガスの流量Ｑｓ’’（ｇ／ｓ）を、真空部４１内に流出した前記測定用ガスの流量とし、この流量（ｇ／ｄａｙに換算）と、ガス透過度測定部４３としての電離真空計（Ｐａ）及び四重極質量分析計（Ａ）のゼロ点を引いた計測値との相関関係から校正用の検量線を得る。図２に、実施例における検量線グラフを示す。 The flow rate Q s ″ (g / s) of the measurement gas flowing out from the conductance unit 28 obtained by the equation (3) is set as the flow rate of the measurement gas flowing out into the vacuum unit 41, and this flow rate (g Calibration curve for the calibration from the correlation between the ionization vacuum gauge (Pa) and the quadrupole mass spectrometer (A) as the gas permeability measuring unit 43 and the measured value obtained by subtracting the zero point. obtain. FIG. 2 shows a calibration curve graph in the example.
　次に、ガスバリアフィルム２を保持させた状態（図１（ｂ）参照）で、ガスバリアフィルム２のガス透過度を測定する。なお、ガスバリアフィルム２としては、ポリエチレンナフタレート（ＰＥＮ）を主材とするハイバリア性のフィルム（試料直径；Φ５０ｍｍ、透過部直径；Φ４０ｍｍ）を用いた。
　先ず、真空ポンプ１７，４２をそれぞれ作動させ、ガス透過度測定装置１内を真空排気させる。次いで、測定用流路２５の開閉弁２６を開け、校正用流路２７の開閉弁２９を閉じた状態で、ガス供給部２１の開閉弁２３を開け、ガス供給部２１から前記測定用ガス（水蒸気）の供給を開始する。水蒸気の暴露条件は、１気圧の大気、４０℃、９０％湿度である。前記測定用ガスは、測定用流路２５を経由してガス暴露側保持部１１側からガス暴露室Ａに流入し、一部がガスバリアフィルム２を透過してガス透過室Ｂ中に流出し、延いては、前記測定用ガス透過側保持部１３側から真空部４１に流出する。ガス透過度測定部４３の計測値が一定となるのを待ち、真空部４１内に流出した前記測定用ガスの流量に関する情報を計測する。 Next, the gas permeability of the gas barrier film 2 is measured in a state where the gas barrier film 2 is held (see FIG. 1B). The gas barrier film 2 was a high barrier film (sample diameter: Φ50 mm, transmission part diameter: Φ40 mm) mainly composed of polyethylene naphthalate (PEN).
First, the vacuum pumps 17 and 42 are operated to evacuate the gas permeability measuring device 1. Next, the on-off valve 26 of the measurement channel 25 is opened, and the on-off valve 23 of the gas supply unit 21 is opened in a state where the on-off valve 29 of the calibration channel 27 is closed. Supply of water vapor) is started. The exposure conditions for water vapor are 1 atmosphere, 40 ° C., and 90% humidity. The measurement gas flows into the gas exposure chamber A from the gas exposure side holding unit 11 side via the measurement flow path 25, and part of the gas passes through the gas barrier film 2 and flows out into the gas transmission chamber B. As a result, it flows out to the vacuum part 41 from the measurement gas permeation side holding part 13 side. Waiting for the measurement value of the gas permeability measuring unit 43 to become constant, information on the flow rate of the measurement gas flowing into the vacuum unit 41 is measured.
　ここで、ガス透過度測定部４３の計測値に基づき、前記校正用の検量線を用いて、ガスバリアフィルム２を透過した前記測定用ガスの流量を定量化し、これによりガスバリアフィルム２のガス透過度を決定する。
　ここで、本実施例のように、ガスバリアフィルム２としてハイバリア性のフィルムを測定対象とする場合には、前記測定用ガスの透過量が極微量となり、装置内に生ずる僅かなガス放出等も、その影響が大きくなることから、ステンレス板などの前記測定用ガスの透過量が無視できる試材をガスバリアフィルム２に代えてフィルム保持室１０に保持させ、その際のガス透過度測定部４３の計測値を取得し、両者の差をとることで、より正確にガスバリアフィルム２のガス透過度を決定することができる。
　ここでは、前記試材としてステンレス板を用い、ガス透過度測定部４３としての電離真空計のガスバリアフィルム２と前記試材の各計測値の差（ΔＰ）をとり、ガスバリアフィルム２のガス透過度を決定することとした。図３に、実施例におけるガス透過度に関する測定グラフを示す。
　なお、図３において、ΔＰは、１．０４×１０－６Ｐａであり、このΔＰと対応する前記校正用の検量線から得られるガス透過量（水蒸気透過量）は、８．０６×１０－６（ｇ／ｄａｙ）であり、そのガス透過度（水蒸気透過度）は、６．４１×１０－３（ｇ／ｄａｙ／ｍ２）であった。 Here, based on the measurement value of the gas permeability measurement unit 43, the calibration gas for calibration is used to quantify the flow rate of the measurement gas that has permeated the gas barrier film 2, and thereby the gas permeability of the gas barrier film 2 is determined. To decide.
Here, as in this example, when a high barrier film is used as the measurement object as the gas barrier film 2, the amount of the measurement gas transmitted is extremely small, and a slight gas release generated in the apparatus is Since the influence is increased, a sample material such as a stainless steel plate that can ignore the amount of the measurement gas permeated is held in the film holding chamber 10 instead of the gas barrier film 2, and the gas permeability measurement unit 43 performs measurement at that time. By acquiring the value and taking the difference between the two, the gas permeability of the gas barrier film 2 can be determined more accurately.
Here, a stainless steel plate is used as the sample, and the difference (ΔP) between the measured values of the gas barrier film 2 of the ionization vacuum gauge as the gas permeability measuring unit 43 and the sample is taken, and the gas permeability of the gas barrier film 2 is taken. It was decided to decide. In FIG. 3, the measurement graph regarding the gas permeability in an Example is shown.
Incidentally, in FIG. 3, [Delta] P is 1.04 × 10 -6 Pa, the gas permeation amount obtained from the calibration curve for the calibration corresponding to the [Delta] P (water vapor transmission amount), 8.06 × 10 - 6 (g / day), and the gas permeability (water vapor permeability) was 6.41 × 10 −3 (g / day / m 2 ).
　以上のように、本発明のガス透過度測定装置は、ガス透過度測定部を取外すことなく、その校正作業を簡素化可能であるとともに、正確にガス透過度を測定可能であるため、用途ごとに様々な特性を有するガスバリアフィルムのガス透過度の測定に広く用いることができる。 As described above, the gas permeability measuring device of the present invention can simplify the calibration work without removing the gas permeability measuring unit and can accurately measure the gas permeability. It can be widely used for measurement of gas permeability of gas barrier films having various characteristics.
　　　１　　　ガス透過度測定装置
　　　２　　　ガスバリアフィルム
　　１０　　　フィルム保持室
　　１１　　　ガス暴露側保持部
　１２，１４　シール部材
　　１３　　　ガス透過側保持部
　　１５　　　排気部
　１６，２３，２４，２６，２９　開閉弁
　１７，４２　真空ポンプ
　　２０　　　ガス上流部
　２１，２２　ガス供給部
　　２５　　　測定用流路
　　２７　　　校正用流路
　　２８　　　コンダクタンス部
　　３０　　　圧力測定部
　　４０　　　ガス下流部
　　４１　　　真空部
　　４３　　　ガス透過度測定部 DESCRIPTION OF SYMBOLS 1 Gas permeability measuring apparatus 2 Gas barrier film 10 Film holding chamber 11 Gas exposure side holding part 12, 14 Seal member 13 Gas permeation side holding part 15 Exhaust part 16, 23, 24, 26, 29 On-off valve 17, 42 Vacuum pump 20 Gas upstream part 21, 22 Gas supply part 25 Measurement flow path 27 Calibration flow path 28 Conductance part 30 Pressure measurement part 40 Gas downstream part 41 Vacuum part 43 Gas permeability measurement part

Claims (4)

  1. 　ガスバリアフィルムのガス暴露面側に配されるガス暴露側保持部と前記ガスバリアフィルムのガス透過面側に配されるガス透過側保持部とで前記ガスバリアフィルムの周部を挟持して保持可能とされ、前記ガスバリアフィルムを保持させたときに、測定用ガスが流入される前記ガス暴露面と前記ガス暴露側保持部とで画成されるガス暴露室、及び、前記ガス透過面から透過する前記測定用ガスが流入される前記ガス透過面と前記ガス透過側保持部とで画成されるガス透過室が形成されるフィルム保持室と、
    　前記測定用ガスを供給するガス供給部、前記ガス供給部－前記ガス暴露側保持部間に配される開閉自在の測定用流路、及び、前記ガス供給部－前記ガス暴露側保持部間に配され、前記測定用流路を閉状態としたとき開状態とされ、前記測定用流路を開状態としたとき閉状態とされるように開閉自在とされ、開状態において前記ガスバリアフィルムを保持しない状態の前記フィルム保持室に流入させる前記測定用ガスの流量を測定可能な校正用測定部を有する校正用流路を備えるガス上流部と、
    　前記ガス透過側保持部と接続される中空の真空部、前記真空部内を排気する真空ポンプ、及び、前記真空部に取付けられ、前記ガスバリアフィルムを保持しない状態の前記フィルム保持室から流出する前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされるとともに、前記ガスバリアフィルムを保持した状態で前記ガス透過室から流出する前記ガスバリアフィルムを透過した前記測定用ガスの流量を前記校正用測定部により校正して測定可能とされるガス透過度測定部を備えるガス下流部と、
    　を有することを特徴とするガス透過度測定装置。     The gas barrier film holding portion disposed on the gas exposure surface side of the gas barrier film and the gas permeation side holding portion disposed on the gas permeation surface side of the gas barrier film can hold and hold the peripheral portion of the gas barrier film. When the gas barrier film is held, the gas exposure chamber defined by the gas exposure surface into which the measurement gas is introduced and the gas exposure side holding portion, and the measurement that is transmitted from the gas transmission surface. A film holding chamber in which a gas permeation chamber defined by the gas permeation surface and the gas permeation side holding portion into which a working gas flows is formed;
    A gas supply unit for supplying the measurement gas, an openable and closable measurement flow channel disposed between the gas supply unit and the gas exposure side holding unit, and between the gas supply unit and the gas exposure side holding unit It is opened and opened when the measurement channel is closed, and can be opened and closed so as to be closed when the measurement channel is opened and holds the gas barrier film in the open state. A gas upstream portion comprising a calibration flow path having a calibration measurement section capable of measuring the flow rate of the measurement gas to be flowed into the film holding chamber in a state of not being,
    A hollow vacuum portion connected to the gas permeation side holding portion, a vacuum pump for exhausting the inside of the vacuum portion, and the measurement attached to the vacuum portion and flowing out from the film holding chamber in a state not holding the gas barrier film The flow rate of the measurement gas transmitted through the gas barrier film flowing out of the gas permeation chamber in a state where the gas barrier film is held can be measured by calibrating the flow rate of the gas by the calibration measurement unit. A gas downstream part equipped with a gas permeability measuring part that can be calibrated and measured by a calibration measuring part;
    A gas permeability measuring apparatus comprising:
  2. 　フィルム保持室に流入される測定用ガスの流入方向に沿ってガス透過側保持部から前記測定用ガスを流出させるとともに、真空部が前記流入方向に沿って中空とされ、前記流入方向の延長位置に真空ポンプが配されるように構成される請求項１に記載のガス透過度測定装置。 The measurement gas is caused to flow out from the gas permeation side holding part along the inflow direction of the measurement gas flowing into the film holding chamber, and the vacuum part is hollow along the inflow direction, and the extended position in the inflow direction The gas permeability measuring device according to claim 1, wherein a vacuum pump is arranged in the gas pump.
  3. 　校正用測定部が、オリフィス、細管及び多孔質体の少なくともいずれかで形成され、コンダクタンスが予め測定されたコンダクタンス部と、前記コンダクタンス部に流入される測定用ガスの圧力を測定する圧力測定部と、を有する請求項１から２のいずれかに記載のガス透過度測定装置。 A calibration measurement unit is formed of at least one of an orifice, a thin tube, and a porous body, and a conductance unit whose conductance is measured in advance, and a pressure measurement unit that measures the pressure of the measurement gas flowing into the conductance unit, The gas permeability measuring device according to claim 1, comprising:
  4. 　コンダクタンス部が、分子流条件を満たす状態で測定用ガスを流通可能とされる請求項３に記載のガス透過度測定装置。 The gas permeability measuring apparatus according to claim 3, wherein the conductance part is capable of circulating the measurement gas in a state where the molecular flow condition is satisfied.
PCT/JP2014/073925 2013-09-19 2014-09-10 Gas permeability measuring device WO2015041115A1 (en)

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