WO2016114003A1 - Dispositif de mesure de la perméabilité au gaz - Google Patents

Dispositif de mesure de la perméabilité au gaz Download PDF

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Publication number
WO2016114003A1
WO2016114003A1 PCT/JP2015/082853 JP2015082853W WO2016114003A1 WO 2016114003 A1 WO2016114003 A1 WO 2016114003A1 JP 2015082853 W JP2015082853 W JP 2015082853W WO 2016114003 A1 WO2016114003 A1 WO 2016114003A1
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Prior art keywords
sample
gas
ring
downstream
upstream
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PCT/JP2015/082853
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English (en)
Japanese (ja)
Inventor
吉田　肇
高橋　善和
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国立研究開発法人産業技術総合研究所
株式会社Ｔｉ
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Application filed by 国立研究開発法人産業技術総合研究所, 株式会社Ｔｉ filed Critical 国立研究開発法人産業技術総合研究所
Priority to JP2016569241A priority Critical patent/JP6337293B2/ja
Publication of WO2016114003A1 publication Critical patent/WO2016114003A1/fr

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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

Definitions

  • the present invention relates to a gas permeability measuring device used for measuring gas permeability of a film sample by a differential pressure method.
  • a differential pressure method is known as a method for measuring the gas permeability of a film member.
  • the differential pressure method after a film sample is mounted in a state of hermetically sealing between two chambers of a gas permeable cell, the low pressure chamber is evacuated and the test gas is introduced into the high pressure chamber.
  • the gas permeability is measured as a pressure increase on the low-pressure side or an increase in gas amount (JIS K 7126-1), or a pressure increase or gas amount on the low-pressure side.
  • the gas adsorption / desorption reaction to the wall of the low-pressure chamber is balanced while the low-pressure chamber is evacuated, and the gas permeation amount in the low-pressure chamber and the exhaust amount of the vacuum pump
  • a method of measuring the gas permeability by measuring the pressure and the like at the time when and become balanced.
  • the gas permeability measuring device for the film member by the differential pressure method include a flange for holding a film, a container for exposing gas to the film, and a side opposite to the gas exposure surface of the film.
  • the conventional gas permeability measuring apparatus has a problem that such a very small gas barrier property cannot be measured with high efficiency and high accuracy in a short time.
  • WVTR Water Vapor Transmission Rate
  • a vacuum vessel which is evacuated by a vacuum pump of pumping speed 0.01 m 3 / s, the introduction of the water vapor flow rate of 1.3 ⁇ 10 -11 Pa ⁇ m 3 / s, the water vapor partial pressure within the vacuum vessel 1.3 ⁇ 10 ⁇ 9 Pa. That is, in order to measure the water vapor permeability on the order of 10 ⁇ 6 g / m 2 / day by the differential pressure method, it is necessary to measure the water vapor partial pressure on the order of 10 ⁇ 9 Pa. In order to measure the extremely small water vapor partial pressure such as 10 ⁇ 9 Pa, the background water vapor partial pressure should be lowered to at least 10 ⁇ 8 Pa, desirably 10 ⁇ 9 Pa or less. Desired.
  • a plurality of processing chambers having independent exhaust systems are brought into and out of a vacuum vessel connected via a gate valve, whereby heat treatment and vapor deposition on the semiconductor wafer are performed under different vacuum conditions for each processing chamber.
  • a load lock device that performs processing or the like is known (see, for example, Patent Document 2). According to such a load lock device, every time a semiconductor wafer is carried into and out of the vacuum container, the entire container is not opened to the atmosphere, and desired processing can be performed in a processing chamber that has been evacuated to high vacuum in advance.
  • An object of the present invention is to solve the above-mentioned problems in the prior art and to provide a gas permeability measuring device capable of measuring the gas permeability of a film sample in a short time, with high efficiency and with high accuracy.
  • Means for solving the problems are as follows. That is, ⁇ 1> A metal sample holder into which the film sample is removably inserted in a state where an opening is formed and both the gas exposure surface and the gas transmission surface of the film sample are exposed from the opening, and one end side is A transfer rod that can be detachably attached to the sample holder, and an insertion portion that allows the transfer rod to be inserted into and retracted from the internal space in an airtight state are formed, and the sample holder can stay in the internal space A sample preparation unit, a sample analysis unit in which the sample holder can be carried in and out in an internal space by the forward and backward movement of the transfer rod, and the sample holder between the sample preparation unit and the sample analysis unit in an open state And a gate valve that can be sealed in a closed state between the sample preparation unit and the sample analysis unit in a closed state.
  • a downstream O-ring holding portion embedded in a state in which a part of the downstream O-ring is in contact with the gas permeable surface of the film sample exposed from the sample holder.
  • a downstream seal member fixed to the inner wall, and an upstream O-ring embedded in a partially protruding state so as to contact the gas exposure surface of the film sample exposed from the sample holder;
  • An upstream O-ring holding portion disposed opposite to the downstream O-ring holding portion so as to be able to sandwich the film sample exposed from the sample holder with the downstream O-ring, and a gas introduction portion connected to a gas supply source The film sample is sandwiched between the upstream O-ring holding portion and the downstream O-ring holding portion, and is separated from the downstream O-ring holding portion.
  • An upstream seal member that is supported by the sample analyzer so that at least the upstream O-ring holding portion can be moved so that the sample holder is inserted between the upstream O-ring and the downstream O-ring.
  • the gas exposure surface of the film sample, the inside of the upstream O-ring, and the inside of the upstream sealing member And a gas permeation measurement chamber defined by the gas permeation surface of the film sample, the inner side of the downstream O-ring, the inner side of the downstream seal member, and the inner wall of the sample analyzer.
  • a first vacuum pump that is connected to the sample preparation unit and evacuates the vacuum vessel, and the downstream seal unit as viewed from the downstream O-ring of the sample analysis unit Is connected to a second vacuum pump that exhausts the inside of the vacuum vessel and a portion that defines the gas permeation amount measurement chamber of the sample analysis unit, and the gas permeation amount from the film sample.
  • a gas permeability measuring apparatus comprising: a gas permeation amount measuring device that measures a permeation amount of a measurement gas that has permeated into a measurement chamber.
  • ⁇ 3> The gas permeability according to any one of ⁇ 1> to ⁇ 2>, wherein a metal plate partially opened is fitted inside a downstream O-ring partly protruding from the downstream seal member. measuring device.
  • ⁇ 4> An upstream O-ring holding portion formed as a thick portion on the outer peripheral side of one surface, and the other surface so that the one surface side is pushed out to the other surface side. Standing on the body, the barrel part moves and moves the upstream side seal member away from the downstream side seal member, and moves the measurement gas from the standing end side while keeping the airtightness inside the sample analysis part.
  • the gas permeability measuring device according to any one of ⁇ 1> to ⁇ 3>, wherein the gas permeability measuring device is formed as an overall substantially disk-like member having a hollow tubular gas introduction portion that can be introduced into the gas.
  • ⁇ 5> The gas permeability measuring apparatus according to any one of ⁇ 1> to ⁇ 4>, wherein a heater for heating the internal space of the sample preparation unit is provided.
  • ⁇ 6> The gas permeability measuring device according to any one of ⁇ 1> to ⁇ 5>, wherein the gas permeability measuring device is provided in a sample preparation unit and includes a stock unit for stocking a sample holder.
  • the present invention it is possible to solve the above-mentioned problems in the prior art, and to provide a gas permeability measuring device capable of measuring the gas permeability of a film sample with high efficiency and high accuracy in a short time.
  • FIG. 4 is a cross-sectional view showing a cross section taken along line AA of FIG. It is explanatory drawing explaining an O-ring. It is explanatory drawing which expands and shows the sealing mechanism of the gas permeability measuring apparatus which concerns on the reference example 1.
  • FIG. It is explanatory drawing which expands and shows the seal mechanism of the gas permeability measuring apparatus which concerns on the modification of the gas permeability measuring apparatus which concerns on the reference example 1.
  • FIG. 1 is an explanatory diagram showing an outline of a gas permeability measuring apparatus according to an embodiment of the present invention.
  • the gas permeability measuring apparatus 100 mainly includes a seal mechanism 1, a sample analysis unit 10, a sample preparation unit 20, a gate valve 30, a transfer rod 31, and a sample holder 32. It is configured.
  • the sample preparation unit 20 includes a vacuum vessel 21, a heater 22, a sample holder stock mechanism 25, and an insertion unit 26.
  • the vacuum vessel 21 is a cylindrical member formed from a known vacuum vessel forming material such as a stainless steel material, and the internal space is a sample preparation chamber 27.
  • an insertion portion 26 is formed for inserting the transfer rod 31 with the sample holder 32 attached thereto into the sample preparation chamber 27 in an airtight state so as to be movable forward and backward.
  • the sample holder 32 can stay in a state where the sample holder 32 is held by a sample holder stock mechanism 25 described later or attached to the transfer rod 31.
  • the vacuum vessel 21 is formed with a sealing door (not shown) on the side surface, and the sample holder 32 is attached to and detached from the transfer rod 31 through the sealing door, and the sample holder 32 is stocked to the sample holder stock mechanism 25 as necessary. It is possible to perform.
  • the other end side of the vacuum vessel 21 is connected to the vacuum vessel 11 of the sample analyzer 10 via the gate valve 30 and is connected to the vacuum vessel 21 with the gate valve 30 closed.
  • 28 enables the inside of the sample preparation chamber 27 to be evacuated independently of the sample analyzer 10.
  • the first vacuum pump 28 can be appropriately selected from known vacuum pumps. However, when a high gas barrier film is to be measured, the inside of the sample preparation chamber 27 is 10 ⁇ 3 Pa or less. For example, a turbo molecular pump or the like can be used.
  • a heater 22 composed of a known heating device is provided.
  • the heater 22 is provided around the outer periphery of the vacuum vessel 21, but the heater 22 may be arranged in another manner or may be arranged in the vacuum vessel 21.
  • the sample holder stock mechanism 25 is arranged in the sample preparation chamber 27, has a stock portion 23 capable of stocking a plurality of sample holders 32, one end connected to the stock portion 23, and the other end side protruding outward of the vacuum vessel 21. And a stock portion support portion 24 formed of a rod-like member that extends while keeping airtightness outside the sample preparation chamber 27.
  • the sample holder stock mechanism 25 can be formed of a known metal material such as stainless steel.
  • the configuration of the sample holder stock mechanism 25 is only an example, and the configuration is not limited to this configuration as long as the sample holder stock mechanism 27 has a stock portion in which the sample holder 32 can be stocked.
  • the sample analyzer 10 includes a vacuum vessel 11.
  • the vacuum vessel 11 is a cylindrical member formed from a known vacuum vessel forming material such as a stainless steel material, and the internal space serves as the sample analysis chamber 12.
  • One end side of the vacuum vessel 11 is connected to the vacuum vessel 21 of the sample preparation unit 20 via the gate valve 30, and the sample is taken by the second vacuum pump 13 connected to the vacuum vessel 11 with the gate valve 30 closed.
  • the inside of the analysis chamber 12 can be exhausted independently of the sample preparation unit 20.
  • the second vacuum pump 13 can be appropriately selected from known vacuum pumps. However, when a high gas barrier film is to be measured, the inside of the sample analysis chamber 12 is set to 10 ⁇ 3 Pa or less. What can exhaust is preferable, for example, a turbo molecular pump can be used.
  • the vacuum container 11 can carry the sample holder 32 in and out of the sample analysis chamber 12 by the forward and backward movement of the transfer rod 31 with the gate valve 30 opened.
  • a part of the inner wall surface of the downstream side seal member 3 is formed so as to form a part of a gas permeation amount measurement chamber 41 to be described later. May not be formed in such a shape.
  • a sample holder support for holding the sample holder 32 carried into the sample analysis chamber 12 as an example is provided at the bottom of the vacuum vessel 11. Part 14 is formed.
  • the vacuum vessel 11 and the vacuum vessel 21 can be formed by connecting separate vacuum vessels using the gate valve 30 as a connecting member, for example.
  • the gate valve 30 is formed of a known metal material such as stainless steel, and is arranged between these parts so as to connect the sample preparation unit 20 (vacuum vessel 21) and the sample analysis unit 10 (vacuum vessel 11).
  • the sample holder 32 can be loaded and unloaded between the sample preparation unit 20 and the sample analysis unit 10 (between the sample preparation chamber 27 and the sample analysis chamber 12), and in the sample preparation unit 20 and the sample analysis in the closed state.
  • the inside of the unit 10 between the sample preparation chamber 27 and the sample analysis chamber 12
  • the transfer rod 31 is a rod-like member whose one end can be detachably attached to the sample holder 32, and those used in a known load lock device can be suitably used.
  • FIG. 2 is an explanatory view showing an enlarged seal mechanism.
  • the seal mechanism 1 includes an upstream seal member 2 and a downstream seal member 3.
  • upstream means close to the supply source gas supply source 6 (see FIG. 1) in the measurement gas flow path
  • downstream means flow of the measurement gas. In the path, it means being far from the source gas supply source 6 (see FIG. 1).
  • the upstream seal member 2 is formed with an upstream O-ring holding portion 2a and a gas introduction portion 2b.
  • the upstream O-ring holding part 2a is embedded in a state in which the upstream O-ring 4a protrudes so that the upstream O-ring 4a comes into contact with the gas exposure surface of the film sample F exposed from the sample holder 32.
  • the film sample F exposed from the sample holder 32 with the O-ring 4b is disposed so as to face the downstream O-ring holding portion 3 ′ so that it can be pinched.
  • the gas introduction part 2 b is connected to the gas supply source 6 and can introduce the measurement gas supplied from the gas supply source 6 into the gas exposure chamber 40 formed inside the upstream seal member 2.
  • the upstream seal member 2 approaches the downstream O-ring holding portion 3 ′ so that the film sample F is sandwiched between the upstream O-ring 4a and the downstream O-ring 4b, and the downstream O-ring holding portion 3 ′.
  • At least the upstream O-ring holding part 4a is supported by the sample analyzer 10 so as to be movable so that the sample holder F is inserted between the upstream O-ring 4a and the downstream O-ring 4b.
  • the entire upstream seal member 2 is movable.
  • upstream side seal member 2 (upstream side O-ring holding part 4a) is moved upstream from the inner wall of the vacuum vessel 11 of the sample analysis part 10 for the purpose of moving and supporting the upstream side seal member 2 with respect to the downstream side seal member 3 in a stable state.
  • a rail member (not shown) that conveys and supports the seal member 2 may be formed.
  • the upstream seal member 2 includes an upstream O-ring holding portion 2a formed as a thick portion on the outer peripheral side of one surface, and the other surface so as to push the one surface side to the other surface side.
  • the body portion is a moving operation unit for separating and approaching the upstream side seal member 2 with respect to the downstream side seal member 3 and standing up while maintaining airtightness in the sample analysis unit 10 (sample analysis chamber 12). It is formed as an overall substantially disk-shaped member having a hollow tubular gas introduction part 2b capable of introducing a measurement gas into the pipe from the end side.
  • the upstream seal member 2 may not have such a configuration.
  • the gas introduction part 2b is a hollow tubular member erected on the other surface so that the one surface side is pushed out to the other surface side, and the upstream O-ring 4a and the downstream O
  • the part is directly operated to perform the moving operation from the outside of the sample analysis unit 10 (sample analysis chamber 12). Instead, a gas is introduced into the opening of the vacuum vessel 11 of the sample analysis unit 10.
  • a pipe joint portion such as a bellows pipe that can move the upstream side seal member 2 through the gas introduction portion 2b while being connected to the introduction portion 2b and being airtight is arranged, thereby indirectly connecting the gas introduction portion 2b. It is good also as making it operate automatically.
  • the upstream seal member 2 can be formed of a known metal material such as stainless steel except for the upstream O-ring 4a.
  • the downstream-side seal member 3 has a downstream-side O-ring holding portion 3 ′ that is embedded in a state in which the downstream-side O-ring 4 b protrudes so that the downstream-side O-ring 4 b comes into contact with the gas permeable surface of the film sample F exposed from the sample holder 32. And fixed to the inner wall of the vacuum vessel 11 of the sample analyzer 10. Further, the downstream seal member 3 is disposed at a position where the sample holder 32 carried into the sample analysis chamber 12 by the movement of the transfer rod 31 and the downstream O-ring 4b abut. Therefore, the film sample F inserted into the sample holder 32 and the downstream O-ring 4b are brought into contact with each other only by moving the transfer rod 31 without adjusting the position of the downstream O-ring 4b.
  • the sample holder 32 can be held between the upstream O-ring 4a and the downstream O-ring 4b only by performing an operation of separating and approaching the upstream sealing member 2 with respect to the downstream sealing member 3. Further, after the measurement, since the sample holder 32 exists at the destination of the transfer rod 31, the sample holder 32 can be attached to one end side of the transfer rod 31 simply by performing the forward operation of the transfer rod 31. The sample holder 32 can be easily collected by the transfer rod 31.
  • the downstream seal member 3 is formed as a substantially disk-shaped member having a downstream O-ring holding portion 3 ′ formed as a thick portion on the outer peripheral side of one surface and having an open center.
  • the downstream seal member 3 can be formed of a known metal material such as stainless steel, except for the downstream O-ring 4b.
  • FIG. 3A is an explanatory diagram for explaining the sample holder portion
  • FIG. 3B is a cross-sectional view taken along the line AA of FIG. 3A
  • FIG. It is explanatory drawing explaining a ring.
  • the sample holder 32 is formed with two metal plates 33a each having a circular opening having a diameter ⁇ 1 at the center and formed of a known metal material such as stainless steel. , 33b, and the metal plates 33a, 33b can be fixed by screws 34a to 34d in a state where the film F is inserted between them, and can be fixed to one surface (gas exposed surface) of the film sample F through the opening. The other surface (gas permeable surface) is exposed. Further, the sample holder 32 is provided with an attachment portion 35 and can be detachably attached to the transfer rod 31 by switch-type fitting between the one end side of the transfer rod 31 and the attachment portion 35 or their magnetic attachment. Is done. Note that the attachment portion 35 is not necessarily provided in the case of magnetic attachment or the like.
  • the upstream and downstream O-rings 4a and 4b are each formed of a known resin material such as fluororubber, or a soft metal material such as indium or gold, and has an outer diameter of ⁇ 2 and an inner diameter of ⁇ 3 ( (See FIG. 4).
  • the outer diameter ⁇ 2 of the upstream and downstream O-rings 4a, 4b is smaller than the diameter ⁇ 1 of the opening of the sample holder 32, and is exposed directly from the sample holder 32 at the upstream and downstream O-rings 4a, b.
  • the film sample F can be sandwiched, and the area surrounded by the inner diameter ⁇ 3 is the gas permeation area of the film sample F.
  • the upstream and downstream O-rings 4a and 4b may have a circular cross-sectional shape when not sealed, but preferably have a square cross-sectional shape from the viewpoint of obtaining high airtightness. .
  • this example is intended to simplify the description, the opening of the sample holder 32, the upstream-side and downstream-side O-ring 4a, if a size larger than the outer diameter [Phi 2 of b, In particular, the upstream and downstream O-rings 4a and 4b do not need to be the same material and the same size as long as the film sample F can be sandwiched.
  • the gas permeability measuring apparatus 100 will be described with reference to FIG. 1 again.
  • the film sample F is sandwiched between the upstream O-ring 4a and the downstream O-ring 4b, the gas exposed surface of the film sample F, the inside of the upstream O-ring 4a, and the upstream seal member 2
  • the gas permeation surface 40 defined by the inside of the gas, the gas permeable surface of the film sample F, the inside of the downstream O-ring 4b, the inside of the downstream seal member 3, and the inner wall of the sample analyzer 10 (vacuum vessel 11).
  • a gas permeation amount measurement chamber 41 to be defined is formed.
  • a metal plate 5 having a part opened inside the downstream O-ring 4 b partially protruding from the downstream seal member 3 is fitted.
  • the film sample F is preferably supported by the metal plate 5. That is, since the pressure in the gas permeation amount measurement chamber 41 is lower than that in the gas exposure chamber 40, the film sample F is drawn toward the gas permeation amount measurement chamber 41, and upstream and downstream due to detachment or bending from the sample folder 32.
  • the metal plate 5 may side O-ring 4a, situations where Estimate the area in gas transmission area of the film sample F surrounded by the inner diameter [Phi 3 of b is generated, the gas permeation side of the film sample F for supporting a metal plate 5 It is preferable.
  • the metal plate 5 a metal plate formed of a known metal material such as stainless steel and having one or a plurality of openings formed in an arbitrary place or a metal plate having openings formed in a mesh shape is used. Can do.
  • the gas permeation amount measuring unit 42 (gas analyzer) is connected to a portion that defines the gas permeation amount measurement chamber 41 of the sample analysis unit 10 (vacuum vessel 11), and enters the gas permeation amount measurement chamber 41 from the film sample F. Measure the amount of permeated gas.
  • transmission amount measurement part 42 Well-known vacuum gauges, such as an ionization vacuum gauge, and well-known mass spectrometers, such as a quadrupole mass spectrometer, can be used.
  • a third vacuum that is connected to a portion that defines the gas permeation amount measurement chamber of the sample analyzer 10 (vacuum vessel 11) and evacuates the gas permeation amount measurement chamber 41 according to the gas permeability measurement method.
  • a pump 43 is arranged. That is, while the gas permeability is evacuated in the gas permeation measurement chamber 41, the gas adsorption / desorption reaction to the inner wall of the gas permeation measurement chamber 41 is balanced, and the gas permeation in the gas permeation measurement chamber 41 is achieved.
  • a third vacuum pump 43 is disposed as the vacuum pump.
  • the third vacuum pump 43 a known vacuum pump can be used.
  • the gas permeation amount measurement chamber 41 can be evacuated to 10 ⁇ 6 Pa or less.
  • a turbo molecular pump or the like can be used. After the inside of the sample analysis chamber 12 is evacuated by the second vacuum pump 13, a gas permeation amount measurement chamber 41 is formed, and the gas permeation amount from the film sample F is increased by the pressure increase or the gas amount in the gas permeation amount measurement chamber 41. In the case of measuring as an increase, the third vacuum pump 43 is not necessarily provided.
  • the gas permeability measuring apparatus 100 concerns on the example which connected the sample preparation part 20 and the sample analysis part 10 to the perpendicular direction, you may connect it to a horizontal direction. In this case, it is preferable to configure the sealing mechanism 1 so that the film sample F is arranged perpendicular to the horizontal plane.
  • the gas permeability measuring apparatus 100 shows one embodiment of the present invention, and the present invention is not limited to this embodiment.
  • the sample analysis chamber 12 is evacuated by the second vacuum pump 13.
  • the sample analysis chamber 12 is evacuated to about 10 ⁇ 3 Pa or less.
  • the sample holder 32 is attached to one end side of the transfer rod 31 that is suspended from the insertion portion 26 into the vacuum container 21 through a sealed door (not shown) of the vacuum container 21.
  • the sample holder 32 is attached to and detached from the transfer rod 31 when the sample holder 32 is attached by the electromagnet of the transfer rod 31, for example, by turning on and off the excitation of the electromagnet.
  • the sample holder 32 attached to the transfer rod 31 may be used by directly attaching one not stocked in the stock portion 23 in the sample holder stock mechanism 25, but from the viewpoint of desorbing adsorbed gas and the like. Those previously stocked in the stock section 23 are preferable.
  • Stock of the sample holder 32 with respect to the stock portion 23 of the sample holder stock mechanism 25 is performed through a sealed door (not shown) of the vacuum vessel 21.
  • the closed door should be closed immediately after the work is completed.
  • water vapor or the like adsorbed on the sample holder 32 or the like retained in the sample preparation chamber 27 is desorbed by heating by the heater 22 and can be efficiently exhausted by the first vacuum pump 28.
  • Heating by the heater 22 is performed at a temperature lower than the heat resistant temperature of the film sample F.
  • the inside of the sample preparation chamber 27 is evacuated to about 10 ⁇ 3 Pa or less.
  • the upstream O-ring 4 a and the downstream side are slid in advance by projecting a portion extending out of the vacuum vessel 11 of the gas introduction portion 2 b of the upstream side seal member 2 or a pipe connected to the portion.
  • the upstream seal member 2 (upstream O-ring holding portion 2a) is separated from the downstream seal member 3 (downstream O-ring holding portion 3 ') so that the sample holder 32 is inserted between the O-ring 4b.
  • the gate valve 30 is opened, and the transfer rod 31 is transported to a predetermined depth in the sample analysis unit 12.
  • a gas exposure chamber 40 defined by the gas exposure surface (one surface) of the film sample F, the inner side of the upstream O-ring 4a, and the inner side of the upstream sealing member 2, It is defined by the gas permeation surface (the other surface opposite to the one surface) of the film sample F, the inside of the downstream O-ring 4b, the inside of the downstream seal member 3, and the inner wall of the sample analyzer 10 (vacuum vessel 11).
  • the formed gas permeation amount measurement chamber 41 is formed in an airtight state.
  • the transfer rod 31 is detached from the sample holder 32, the transfer rod 31 is returned to the sample preparation chamber 27, the gate valve 30 is closed again, and the inside of the sample analysis chamber 12 is subsequently evacuated by the second vacuum pump 13, and the gas is discharged. Complete the measurement preparation for transmission measurement.
  • the measurement is supplied from the gas supply source 6 via the gas introduction part 2b of the upstream side seal member 2 while the gas permeation amount measurement chamber 41 is evacuated by the third vacuum pump.
  • Gas is introduced into the gas exposure chamber 40 and the permeation amount of the measurement gas permeating from the film sample F into the gas permeation amount measurement chamber 41 is measured by a permeation amount gas permeation amount measurement unit 42 (gas analyzer). Do it.
  • the gas adsorption / desorption reaction on the inner wall of the gas permeation amount measurement chamber 41 is in equilibrium, and the gas permeation amount in the gas permeation amount measurement chamber 41 and the exhaust amount of the third vacuum pump 43 are in equilibrium.
  • the gas permeability is measured by measuring the pressure at the time point.
  • the film sample F is a high barrier film
  • the gas permeation amount measurement chamber 41 is evacuated to about 10 ⁇ 6 Pa or less using a third vacuum pump.
  • the film sample F is not exposed to the atmosphere every time the film sample F is carried in and out of the apparatus, and the gas permeation is performed in the sample analyzer 10 that has been evacuated to a desired vacuum environment in advance.
  • the vacuum environment under the measurement conditions can be obtained in a short time, and as a result, the gas permeability of the film sample F can be measured efficiently in a short time. Further, since the gas adsorbed on the film sample F, the sample holder 32, etc.
  • the sample analysis unit 10 can be eliminated in advance by the sample preparation unit 20 before the gas permeability measurement, the sample analysis unit 10 does not desorb them and the measurement conditions can be measured in a short time.
  • the gas permeability of the film sample F can be measured efficiently in a short time.
  • the sample holder 32 in the sample holder stock mechanism 25 in the sample preparation unit 20 the sample holder 32 from which the gas, water vapor, etc. adsorbed on the sample holder 32 are excluded can be prepared in advance. Therefore, the sample analysis unit 10 can obtain a vacuum environment under measurement conditions in a shorter time, and by extension, the gas permeability of the film sample F can be efficiently measured in a short time.
  • the upstream and downstream O-rings 4a and 4b having an outer diameter ⁇ 2 smaller than the opening diameter ⁇ 1 of the metal sample holder 32 are directly provided in the apparatus. Since the gas permeability measurement is performed by holding the sample holder 32, it is possible to measure the gas permeability with high accuracy. As a result, a high barrier film sample of 10 ⁇ 6 g / m 2 / day can be obtained. It can be a measurement object.
  • FIGS. 2 and 5 to 7 in comparison with the gas permeability measuring apparatus according to Reference Examples 1 and 2 below.
  • 5 is an explanatory diagram showing an enlarged seal mechanism of the gas permeability measuring device according to Reference Example 1, and FIG.
  • FIG. 6 is a gas permeation according to a modification of the gas permeability measuring device according to Reference Example 1.
  • FIG. 7 is an explanatory diagram showing an enlarged seal mechanism of the gas measuring device, and
  • FIG. 7 is an explanatory diagram showing an enlarged gas permeability measuring device seal mechanism according to Reference Example 2.
  • the gas permeability measuring apparatus according to the reference example 1, as shown in FIG. 5, the upstream-side and downstream-side O-ring 4a, the outer diameter [Phi 2 of b, the diameter [Phi 1 is smaller metal samples of the opening It is different from the gas permeability measuring apparatus 100 in that the holder 50 is used and the gas sample is measured by holding the film sample F with the metal plates 51a and 51b of the sample holder 50.
  • Reference numeral 53 denotes an attachment portion to the transfer rod 31.
  • the gas permeability measurement apparatus When the gas permeability measurement apparatus according to Reference Example 1 performs the gas permeability measurement, the measurement gas introduced from the gas introduction portion 2b is not sealed by the O-ring, so that the gap between the metal plate 51a and the film sample F is not measured. From the metal plate 51b and the film sample F to the gas permeation amount measurement chamber side (see the black arrow in FIG. 5), and the gas that has permeated the film sample F (see FIG. 5). 5), the gas permeability measurement of the film sample F cannot be performed with high accuracy.
  • O-rings 52a and 52b are embedded in opposing surfaces of the metal plates 51a and 51b, and these O-rings 52a are embedded.
  • B, the O-rings 52a, b are carried into and out of the apparatus together with the sample holder 50 even when the film sample F is held between the metal plate 51b and the film sample. Leaks into the gas permeation measuring chamber side from between F (see the black arrow in FIG. 6), mixes with the gas that has permeated through the film sample (see the white arrow in FIG. 6), and passes through the gas through the film sample F. The degree measurement cannot be performed with high accuracy.
  • a metal sample in which the diameter ⁇ 1 of the opening is smaller than the outer diameter ⁇ 2 of the upstream and downstream O-rings 4 a and 4 b. It is different from the gas permeability measuring apparatus 100 in that the holder 60 is used and the gas sample is measured by holding the film sample F between the metal plates 61a and 61b of the sample holder 60. Moreover, it differs from the gas permeability measuring apparatus according to Reference Example 1 in that a metal plate 61a having a smaller size than the metal plate 51a is used and only the metal plate 61b is sandwiched between the upstream and downstream O-rings 4a and 4b. .
  • Reference numeral 63 denotes an attachment portion to the transfer rod 31.
  • the gas permeability measuring apparatus according to Reference Example 2 does not leak into the sample analysis chamber 12, but the measuring gas is a metal. Since it directly reaches the joint surface between the plate 61b and the film sample F, and this joint surface is not sealed with an O-ring, the measurement gas passes through between the metal plate 61b and the film sample F. It leaks out to the quantity measuring chamber side (see black arrow in FIG. 7), mixes with the gas that has passed through the film sample (see white arrow in FIG. 7), and the gas permeability cannot be measured accurately.
  • the gas permeability measuring apparatus 100 there is no leakage to the gas permeation amount measurement chamber side of the measurement gas, and only the gas that has passed through the film sample F can be measured (white in FIG. 2).
  • the gas permeability measurement of the film sample F can be performed with high accuracy.

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  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

Le problème à résoudre dans le cadre de la présente invention consiste à fournir un dispositif de mesure de la perméabilité au gaz qui permet une mesure très précise et rapide de la perméabilité au gaz d'un échantillon de film. La solution consiste en un dispositif de mesure de la perméabilité au gaz qui est pourvu d'un mécanisme d'étanchéité configuré à partir d'un élément d'étanchéité aval ayant une partie de maintien de joint torique aval dans lequel est enfoncé un joint torique aval et à partir d'un élément d'étanchéité amont dans lequel est formée, par exemple, une partie de maintien de joint torique amont dans laquelle est enfoncé un joint torique amont et qui est disposée de sorte à s'opposer à la partie de maintien de joint torique aval de telle sorte que le joint torique amont et le joint torique aval puissent prendre en sandwich un échantillon de film qui fait saillie depuis un porte-échantillon et qui provoque le déplacement de la partie de maintien de joint torique amont de sorte à s'approcher de la partie de maintien de joint torique aval de telle sorte que l'échantillon de film soit maintenu par le joint torique amont et le joint torique aval et de sorte à se séparer de la partie de maintien de joint torique aval de sorte à insérer le porte-échantillon entre le joint torique amont et le joint torique aval, le mécanisme d'étanchéité étant tel qu'une chambre d'exposition à un gaz et une chambre de mesure de la perméabilité au gaz soient formées dans un état dans lequel le joint torique amont et le joint torique aval prennent en sandwich l'échantillon de film.
PCT/JP2015/082853 2015-01-15 2015-11-24 Dispositif de mesure de la perméabilité au gaz WO2016114003A1 (fr)

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JP2016161527A (ja) * 2015-03-05 2016-09-05 埼玉県 試料の水蒸気透過度測定装置及び水蒸気透過度測定方法
WO2018155678A1 (fr) * 2017-02-27 2018-08-30 国立研究開発法人産業技術総合研究所 Dispositif d'évaluation de propriétés de barrière contre les gaz et procédé d'évaluation des propriétés de barrière contre les gaz
CN109813643A (zh) * 2019-01-01 2019-05-28 中国人民解放军63653部队 一种混凝土及其表面覆膜涂层材料的气体渗透率测量方法
KR20200055185A (ko) * 2018-11-12 2020-05-21 삼성디스플레이 주식회사 수분투습도 측정장치
WO2022023050A1 (fr) * 2020-07-28 2022-02-03 Robert Bosch Gmbh Dispositif et procédé de détermination d'une caractéristique de perméation de gaz d'une couche de matériau
KR102632280B1 (ko) * 2023-04-28 2024-02-02 한국표준과학연구원 이중 실링 및 배기 구조를 포함하는 시료홀더

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JP2016161527A (ja) * 2015-03-05 2016-09-05 埼玉県 試料の水蒸気透過度測定装置及び水蒸気透過度測定方法
JP7041665B2 (ja) 2017-02-27 2022-03-24 国立研究開発法人産業技術総合研究所 ガスバリア性評価装置およびガスバリア性評価方法
KR20190123722A (ko) * 2017-02-27 2019-11-01 고쿠리츠켄큐카이하츠호진 상교기쥬츠 소고켄큐쇼 가스 배리어성 평가 장치 및 가스 배리어성 평가 방법
JPWO2018155678A1 (ja) * 2017-02-27 2020-01-16 国立研究開発法人産業技術総合研究所 ガスバリア性評価装置およびガスバリア性評価方法
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KR102497995B1 (ko) 2017-02-27 2023-02-10 고쿠리츠켄큐카이하츠호진 상교기쥬츠 소고켄큐쇼 가스 배리어성 평가 장치 및 가스 배리어성 평가 방법
KR20200055185A (ko) * 2018-11-12 2020-05-21 삼성디스플레이 주식회사 수분투습도 측정장치
KR102538826B1 (ko) 2018-11-12 2023-06-02 삼성디스플레이 주식회사 수분투습도 측정장치
CN109813643A (zh) * 2019-01-01 2019-05-28 中国人民解放军63653部队 一种混凝土及其表面覆膜涂层材料的气体渗透率测量方法
CN109813643B (zh) * 2019-01-01 2021-06-08 中国人民解放军63653部队 一种混凝土及其表面覆膜涂层材料的气体渗透率测量方法
WO2022023050A1 (fr) * 2020-07-28 2022-02-03 Robert Bosch Gmbh Dispositif et procédé de détermination d'une caractéristique de perméation de gaz d'une couche de matériau
KR102632280B1 (ko) * 2023-04-28 2024-02-02 한국표준과학연구원 이중 실링 및 배기 구조를 포함하는 시료홀더

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