JP6337293B2 - Gas permeability measuring device - Google Patents
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- 230000035699 permeability Effects 0.000 title claims description 80
- 238000011144 upstream manufacturing Methods 0.000 claims description 78
- 238000005259 measurement Methods 0.000 claims description 68
- 238000002360 preparation method Methods 0.000 claims description 38
- 238000012546 transfer Methods 0.000 claims description 31
- 230000007246 mechanism Effects 0.000 claims description 30
- 239000002184 metal Substances 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 238000007789 sealing Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003780 insertion Methods 0.000 claims description 6
- 230000037431 insertion Effects 0.000 claims description 6
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 204
- 239000010408 film Substances 0.000 description 86
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 230000004888 barrier function Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 239000007769 metal material Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229920001973 fluoroelastomer Polymers 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
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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
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
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- General Health & Medical Sciences (AREA)
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Description
本発明は、差圧法によるフィルム試料のガス透過度測定に用いられるガス透過度測定装置に関する。 The present invention relates to a gas permeability measuring device used for measuring gas permeability of a film sample by a differential pressure method.
フィルム部材のガス透過度を測定する方法として差圧法が知られている。前記差圧法としては、フィルム試料を、ガス透過セルの二つのチャンバ間に密封シールするような状態で装着した後、低圧チャンバを真空排気し、試験ガスを高圧チャンバに導入すると、ガスが試験片を通過し、低圧チャンバ内に透過することを利用し、ガス透過度を低圧側の圧力上昇又はガス量の増加として測定する方法（ＪＩＳ Ｋ ７１２６−１）や、低圧側の圧力上昇又はガス量の増加として測定することに代え、前記低圧チャンバを真空排気しつつ、前記低圧チャンバ壁面への気体の吸脱着反応が平衡で、かつ、前記低圧チャンバ内でのガス透過量と真空ポンプの排気量とが平衡となった時点における圧力等を計測してガス透過度を測定する方法により実施される。
前記差圧法による前記フィルム部材の前記ガス透過度測定装置としては、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）。A differential pressure method is known as a method for measuring the gas permeability of a film member. In 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. Instead of measuring as an increase in the pressure, 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 This is carried out by a method of measuring the gas permeability by measuring the pressure and the like at the time when and become balanced.
Examples of 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 gas permeability of the gas permeated from the gas permeable surface into the vacuum portion by a mass spectrometer connected to the vacuum portion capable of exhausting to a predetermined pressure with respect to the gas permeable surface. Has been proposed (see Patent Document 1).
しかしながら、有機ＥＬ、薄膜太陽電池等の半導体分野では、前記フィルム部材に対し、素子内部等への空気等の侵入を抑制するための封止材として１０−６ｇ／ｍ２／ｄａｙ程度のガスバリア性が求められており、従来の前記ガス透過度測定装置では、こうした極微小なガスバリア性を短時間、高効率かつ高精度に測定することができない問題がある。
今、一般的に用いられるサイズである縦横９０ｍｍのフィルム試料を考えたとき、１０−６ｇ／ｍ２／ｄａｙの水蒸気透過度（ＷＶＴＲ；Ｗａｔｅｒ Ｖａｐｏｕｒ Ｔｒａｎｓｍｉｓｓｉｏｎ Ｒａｔｅ）は、１．３×１０−１１Ｐａ・ｍ３／ｓの水蒸気流量に対応する。排気速度０．０１ｍ３／ｓの真空ポンプで真空排気された真空容器に、１．３×１０−１１Ｐａ・ｍ３／ｓの前記水蒸気流量を導入すると、前記真空容器内の水蒸気分圧は、１．３×１０−９Ｐａとなる。即ち、前記差圧法で、１０−６ｇ／ｍ２／ｄａｙ台の前記水蒸気透過度を測定するためには、１０−９Ｐａ台の前記水蒸気分圧を測定する必要が生じる。そして、１０−９Ｐａ台といった極微小の前記水蒸気分圧を測定するためには、バックグラウンドの前記水蒸気分圧を、少なくとも１０−８Ｐａ台、望ましくは１０−９Ｐａ台以下まで下げることが求められる。However, in the field of semiconductors such as organic EL and thin film solar cells, a gas barrier of about 10 −6 g / m 2 / day is used as a sealing material for suppressing the intrusion of air or the like into the element inside the film member. Therefore, 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.
Considering a film sample having a length and width of 90 mm, which is a commonly used size, a water vapor transmission rate (WVTR) of 10 −6 g / m 2 / day is 1.3 × 10 −11. This corresponds to a water vapor flow rate of Pa · m 3 / s. 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, preferably 10 −9 Pa or less. Desired.
一方で、水蒸気は、吸着性・凝集性があることから、不活性ガスに比べて、真空排気しにくいことが知られており、前記真空容器の内璧に吸着した水蒸気は、室温条件下で１０−２Ｐａ程度以下の真空環境下では、おおよそ時間ｔの逆数ｔ−１に従って圧力降下する（例えば、非特許文献１参照）。下記表１に、時間ｔ＝０秒における初期水蒸気分圧と、逆数ｔ−１に従って圧力降下することを仮定して計算した、１０−９Ｐａ台の前記水蒸気分圧を得るまでに要する時間を示す。即ち、１０−９Ｐａ台の前記水蒸気分圧を短時間で得るためには、前記初期水蒸気分圧を下げることが重要であり、そのための機構を開発する必要がある。On the other hand, it is known that water vapor is difficult to evacuate compared to inert gas because it has adsorptive and cohesive properties, and water vapor adsorbed on the inner wall of the vacuum vessel In a vacuum environment of about 10 −2 Pa or less, the pressure drops approximately according to the inverse t −1 of time t (see, for example, Non-Patent Document 1). Table 1 below shows the time required to obtain the water vapor partial pressure on the order of 10 −9 Pa calculated on the assumption that the initial water vapor partial pressure at time t = 0 seconds and the pressure drop according to the reciprocal t −1. Show. That is, in order to obtain the water vapor partial pressure on the order of 10 −9 Pa in a short time, it is important to lower the initial water vapor partial pressure, and it is necessary to develop a mechanism for that purpose.
なお、一般に、１０−９Ｐａ台の前記水蒸気分圧を短時間で得るためには、２００℃以上で真空容器を加熱脱ガス（ベーキング）することが有効である。しかし、測定対象となるフィルム部材の耐熱温度は、典型的には８０℃であるため、前記フィルム部材を前記真空容器に入れた状態で、２００℃以上という高温でのベーキングを行うことができない。In general, in order to obtain the water vapor partial pressure on the order of 10 −9 Pa in a short time, it is effective to heat and degas (bake) the vacuum vessel at 200 ° C. or higher. However, since the heat resistant temperature of the film member to be measured is typically 80 ° C., baking at a high temperature of 200 ° C. or higher cannot be performed in a state where the film member is placed in the vacuum vessel.
ところで、独立した排気系を有する複数の処理室がゲートバルブを介して連設された真空容器に半導体ウエハを搬出入させることで、処理室ごとに異なる真空条件で前記半導体ウエハに対する加熱処理や蒸着処理等を行うロードロック装置が知られている（例えば、特許文献２参照）。こうしたロードロック装置によれば、半導体ウエハを真空容器に搬出入する度、容器全体を大気に開放することがなく、予め高真空に排気された処理室で所望の処理を実施することができる。
しかしながら、こうしたロードロック装置の機構に基づく前記フィルム部材のガス透過度を測定する方法としては、これまで何ら検討されておらず、１０−６ｇ／ｍ２／ｄａｙといったハイガスバリア性のものを含め、前記フィルム試料のガス透過度を短時間、高効率かつ高精度に測定するためには、新たな機構の開発が求められる。By the way, 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.
However, as a method for measuring the gas permeability of the film member based on the mechanism of such a load lock device, nothing has been studied so far, including a high gas barrier property such as 10 −6 g / m 2 / day. In order to measure the gas permeability of the film sample in a short time with high efficiency and high accuracy, development of a new mechanism is required.
本発明は、従来技術における前記諸問題を解決し、短時間、高効率かつ高精度にフィルム試料の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。 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.
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＞ 開口部が形成され、前記開口部からフィルム試料のガス暴露面及びガス透過面の両面が露出する状態で前記フィルム試料が挿脱自在に内挿される金属製の試料ホルダと、一端側が前記試料ホルダと脱着自在に取着可能とされるトランスファーロッドと、前記トランスファーロッドを内部空間に気密状態で進退動自在として挿通させる挿通部が形成されるとともに前記試料ホルダが前記内部空間に滞留可能とされる試料準備部と、前記トランスファーロッドの進退動により内部空間で前記試料ホルダが搬出入可能とされる試料分析部と、開状態で前記試料準備部内−前記試料分析部内間で前記試料ホルダが搬出入可能とされ、閉状態で前記試料準備部内−前記試料分析部内間を気密状態で密閉可能とされるゲート弁とを有する真空容器部と、下流側Ｏリングが前記試料ホルダから露出する前記フィルム試料の前記ガス透過面と当接するよう一部が突出した状態で埋設される下流側Ｏリング保持部を有し、前記試料分析部の内壁に固定される下流側シール部材と、上流側Ｏリングが前記試料ホルダから露出する前記フィルム試料の前記ガス暴露面と当接するよう一部が突出した状態で埋設され、前記上流側Ｏリングと前記下流側Ｏリングとで前記試料ホルダから露出する前記フィルム試料を狭持可能に前記下流側Ｏリング保持部と対向配置される上流側Ｏリング保持部及びガス供給源と接続されるガス導入部が形成され、前記下流側Ｏリング保持部に接近させて前記上流側Ｏリングと前記下流側Ｏリングとで前記フィルム試料を狭持させ、前記下流側Ｏリング保持部から離間させて前記上流側Ｏリングと前記下流側Ｏリングとの間に前記試料ホルダを挿通させるように少なくとも前記上流側Ｏリング保持部を移動可能として前記試料分析部に支持される上流側シール部材とで構成され、前記上流側Ｏリングと前記下流側Ｏリングとで前記フィルム試料を狭持した状態で、前記フィルム試料の前記ガス暴露面と前記上流側Ｏリングの内側と前記上流側シール部材の内側とで画成されるガス暴露室及び前記フィルム試料の前記ガス透過面と前記下流側Ｏリングの内側と前記下流側シール部材の内側と前記試料分析部の内壁で画成されるガス透過量測定室を形成するシール機構と、前記試料準備部と接続され、前記真空容器内を排気する第１の真空ポンプと、前記試料分析部の前記下流側Ｏリングからみて前記下流側シール部材の外側の位置に接続され、前記真空容器内を排気する第２の真空ポンプと、前記試料分析部の前記ガス透過量測定室を画成する部分と接続され、前記フィルム試料から前記ガス透過量測定室内に透過した測定用ガスの透過量を測定するガス透過量計測器と、を備えることを特徴とするガス透過度測定装置。
＜２＞ 更に、試料分析部のガス透過量測定室を画成する部分と接続され、前記ガス透過量測定室内を排気する第３の真空ポンプを備える前記＜１＞に記載のガス透過度測定装置。
＜３＞ 下流側シール部材から一部が突出する下流側Ｏリングの内側に一部が開口された金属板が嵌着される前記＜１＞から＜２＞のいずれかに記載のガス透過度測定装置。
＜４＞ 上流側シール部材が、一の面の外周側に厚肉の部として形成される上流側Ｏリング保持部と、前記一の面側を他の面側に押し出すように前記他の面上に立設され、胴部が前記上流側シール部材の下流側シール部材に対する離間移動及び接近移動の移動操作部をなすとともに試料分析部内の気密を取りつつ立設端側から測定用ガスを管内に導入可能な中空管状のガス導入部とを有する全体略円盤状部材として形成される前記＜１＞から＜３＞のいずれかに記載のガス透過度測定装置。
＜５＞ 試料準備部の内部空間を加熱するヒータが配設される前記＜１＞から＜４＞のいずれかに記載のガス透過度測定装置。
＜６＞ 試料準備部内に配され、試料ホルダをストックするストック部を有する前記＜１＞から＜５＞のいずれかに記載のガス透過度測定装置。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 the 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 A vacuum vessel having a gate valve which can be carried in and out and can be hermetically sealed 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. In the state where the film sample is held 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.
<2> The gas permeability measurement according to <1>, further including a third vacuum pump connected to a portion defining a gas permeation amount measurement chamber of the sample analysis unit and exhausting the gas permeation amount measurement chamber. apparatus.
<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.
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、短時間、高効率かつ高精度にフィルム試料の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。 ADVANTAGE OF THE INVENTION According to this invention, the said various problems in a prior art can be solved, and the gas permeability measuring apparatus which can measure the gas permeability of a film sample with high efficiency and high precision for a short time can be provided.
本発明の一実施形態に係るガス透過度測定装置を図面を参照しつつ説明する。
図１は、本発明の一実施形態に係るガス透過度測定装置の概要を示す説明図である。
該図１に示すように、ガス透過度測定装置１００は、主として、シール機構１と、試料分析部１０と、試料準備部２０と、ゲート弁３０と、トランスファーロッド３１と、試料ホルダ３２とを有して構成される。A gas permeability measuring apparatus according to an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is an explanatory diagram showing an outline of a gas permeability measuring apparatus according to an embodiment of the present invention.
As shown in FIG. 1, 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.
試料準備部２０は、真空容器２１と、ヒータ２２と、試料ホルダストック機構２５と、挿通部２６とを有する。
真空容器２１は、ステンレス鋼材等の公知の真空容器形成材料から形成される筒状部材であり、内部空間が試料準備室２７とされる。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.
真空容器２１の一端側には、試料ホルダ３２が取着された状態のトランスファーロッド３１を試料準備室２７内に気密状態で進退動自在として挿通させる挿通部２６が形成されるとともに、真空容器２１は、試料準備室２７内において、試料ホルダ３２が後述の試料ホルダストック機構２５に保持された状態、或いは、トランスファーロッド３１に取着された状態で滞留可能とされる。
また、真空容器２１は、側面に図示しない密閉扉が形成され、前記密閉扉を通じてトランスファーロッド３１に対する試料ホルダ３２の脱着操作や、必要に応じて、試料ホルダストック機構２５に対する試料ホルダ３２のストック操作を行うことが可能とされる。
また、真空容器２１の他端側は、ゲート弁３０を介して試料分析部１０の真空容器１１と連結され、ゲート弁３０を閉じた状態で、真空容器２１に接続される第１の真空ポンプ２８により試料準備室２７内が試料分析部１０と独立して排気可能とされる。
なお、第１の真空ポンプ２８としては、公知の真空ポンプから適宜選択して用いることができるが、ハイガスバリア性のフィルムを測定対象とする場合、試料準備室２７内を、 １０−３Ｐａ以下に排気可能なものが好ましく、例えば、ターボ分子ポンプ等を用いることができる。On one end side of the vacuum vessel 21, 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. In the sample preparation chamber 27, 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.
Further, 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, but 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.
また、真空容器２１の外周には、試料準備室２７に導入される試料ホルダ３２に吸着された水蒸気等を脱離させ、第１の真空ポンプ２８でより効率的に排気可能とする等の観点から、公知の加熱装置で構成されるヒータ２２が周設される。
なお、本例では、ヒータ２２が真空容器２１の外周に周設されるが、ヒータ２２としては、別の態様で配してもよく真空容器２１内に配されていてもよい。In addition, water vapor or the like adsorbed by the sample holder 32 introduced into the sample preparation chamber 27 is desorbed on the outer periphery of the vacuum vessel 21 so that the first vacuum pump 28 can exhaust more efficiently. Therefore, a heater 22 composed of a known heating device is provided.
In this example, 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.
試料ホルダストック機構２５は、試料準備室２７内に配され、複数の試料ホルダ３２をストック可能なストック部２３と、一端がストック部２３と連結され、他端側が真空容器２１の外方に突出して試料準備室２７外に気密を取りつつ延在する棒状部材で形成されるストック部支持部２４とで構成される。なお、試料ホルダストック機構２５としては、ステンレス鋼等の公知の金属材料で形成することができる。
ただし、この試料ホルダストック機構２５の構成は、一例を示すものであり、試料準備室２７内に試料ホルダ３２をストック可能なストック部を有する構成であれば、こうした構成に限定されない。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.
However, 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.
試料分析部１０は、真空容器１１で構成される。
真空容器１１は、ステンレス鋼材等の公知の真空容器形成材料から形成される筒状部材であり、内部空間が試料分析室１２とされる。
真空容器１１の一端側は、ゲート弁３０を介して試料準備部２０の真空容器２１と連結され、ゲート弁３０を閉じた状態で、真空容器１１に接続される第２の真空ポンプ１３により試料分析室１２内が試料準備部２０と独立して排気可能とされる。
なお、第２の真空ポンプ１３としては、公知の真空ポンプから適宜選択して用いることができるが、ハイガスバリア性のフィルムを測定対象とする場合、試料分析室１２内を１０−３Ｐａ以下に排気可能なものが好ましく、例えば、ターボ分子ポンプ等を用いることができる。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 a measurement target, 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.
また、真空容器１１は、ゲート弁３０を開いた状態で、トランスファーロッド３１の進退動により試料分析室１２内での試料ホルダ３２の搬出入が可能とされる。
真空容器１１の側面では、後述するガス透過量測定室４１の一部を構成するよう、下流側シール部材３の内側の一部壁面が外方に突出するよう形成されるが、真空容器１１としては、このような形状で形成されなくともよい。
また、試料分析室１２内に搬入された試料ホルダ３２を安定的に支持するため、真空容器１１の底部には、一例として試料分析室１２内に搬入された試料ホルダ３２を保持する試料ホルダ支持部１４が形成される。
なお、真空容器１１と真空容器２１とは、例えば、ゲート弁３０を連結部材として別々の真空容器を連結させて形成することができる。In addition, 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.
On the side surface of the vacuum vessel 11, 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.
In addition, in order to stably support the sample holder 32 carried into the sample analysis chamber 12, 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.
ゲート弁３０は、ステンレス鋼等の公知の金属材料で形成され、試料準備部２０（真空容器２１）と試料分析部１０（真空容器１１）とを連結するように、これらの部間に配され、開状態で試料準備部２０内−試料分析部１０内間（試料準備室２７−試料分析室１２間）で試料ホルダ３２が搬出入可能とされ、閉状態で試料準備部２０内−試料分析部１０内間（試料準備室２７−試料分析室１２間）を気密状態で密封可能とされる。
また、トランスファーロッド３１は、一端側が試料ホルダ３２と脱着自在に取着可能とされる棒状部材であり、公知のロードロック装置で用いられるものを好適に使用することができる。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) in the open state, 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) can be sealed in an airtight state.
Further, 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.
シール機構１を図２を参照しつつ説明をする。図２は、シール機構を拡大して示す説明図である。
該図２に示すように、シール機構１は、上流側シール部材２と下流側シール部材３とで構成される。なお、本明細書において、「上流」とは、測定用ガスの流通経路において、供給元のガス供給源６（図１参照）に近いことを指し、「下流」とは、測定用ガスの流通経路において、供給元のガス供給源６（図１参照）から遠いことを指す。The sealing mechanism 1 will be described with reference to FIG. FIG. 2 is an explanatory view showing an enlarged seal mechanism.
As shown in FIG. 2, the seal mechanism 1 includes an upstream seal member 2 and a downstream seal member 3. In this specification, “upstream” means close to the supply source gas supply source 6 (see FIG. 1) in the measurement gas flow path, and “downstream” means flow of the measurement gas. In the path, it means being far from the source gas supply source 6 (see FIG. 1).
上流側シール部材２には、上流側Ｏリング保持部２ａと、ガス導入部２ｂとが形成される。
上流側Ｏリング保持部２ａは、上流側Ｏリング４ａが試料ホルダ３２から露出するフィルム試料Ｆのガス暴露面と当接するよう一部が突出した状態で埋設され、上流側Ｏリング４ａと下流側Ｏリング４ｂとで試料ホルダ３２から露出するフィルム試料Ｆを狭持可能に下流側Ｏリング保持部３’と対向配置される。
また、ガス導入部２ｂは、ガス供給源６と接続され、ガス供給源６から供給される測定用ガスを上流側シール部材２内側に形成されるガス暴露室４０に導入可能とされる。
また、上流側シール部材２は、下流側Ｏリング保持部３’に接近させて上流側Ｏリング４ａと下流側Ｏリング４ｂとでフィルム試料Ｆを狭持させ、下流側Ｏリング保持部３’から離間させて上流側Ｏリング４ａと下流側Ｏリング４ｂとの間に試料ホルダＦを挿通させるように少なくとも上流側Ｏリング保持部４ａを移動可能として試料分析部１０に支持される。なお、ここでは、上流側シール部材２全体が移動可能とされる。また、上流側シール部材２（上流側Ｏリング保持部４ａ）を下流側シール部材３に対して安定状態で移動させ、支持することを目的として、試料分析部１０の真空容器１１内壁に上流側シール部材２を搬送し支持するレール部材（不図示）が形成されていてもよい。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.
Further, 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.
Further, 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. Here, the entire upstream seal member 2 is movable. Further, the 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.
上流側シール部材２は、一の面の外周側に厚肉の部として形成される上流側Ｏリング保持部２ａと、前記一の面側を他の面側に押し出すように前記他の面上に立設され、胴部が上流側シール部材２の下流側シール部材３に対する離間移動及び接近移動の移動操作部をなすとともに試料分析部１０（試料分析室１２）内の気密を取りつつ立設端側から測定用ガスを管内に導入可能な中空管状のガス導入部２ｂとを有する全体略円盤状部材として形成される。
これにより、ガス導入部２ｂの真空容器１１外に突出して延在する部分又は当該部分と接続される配管をスライド操作させて、試料分析室１２内と気密を取りつつ上流側シール部材２を下流側シール部材３側に容易に移動させることができる。ただし、上流側シール部材２としては、このような構成でなくともよい。例えば、本例では、ガス導入部２ｂを前記一の面側を他の面側に押し出すように前記他の面上に立設された中空管状の部材とし、上流側Ｏリング４ａと下流側Ｏリング４ｂとでフィルム試料Ｆを狭持した状態で一部が試料分析部１０（試料分析室１２）内と気密を取りつつ試料分析部１０（試料分析室１２）外に突出して延在させ、該一部を直接操作して試料分析部１０（試料分析室１２）外部からの前記移動操作を行うこととしているが、これに代えて、試料分析部１０の真空容器１１の開口部分に、ガス導入部２ｂと接続され気密を取りつつ上流側シール部材２をガス導入部２ｂを介して前記移動操作させることが可能なベローズ配管等の管継手部を配し、これによりガス導入部２ｂを間接的に操作させることとしてもよい。
なお、上流側シール部材２としては、上流側Ｏリング４ａを除き、ステンレス鋼等の公知の金属材料で形成することができる。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.
As a result, a portion of the gas introduction portion 2b that protrudes outside the vacuum vessel 11 or a pipe connected to the portion is slid to keep the upstream seal member 2 downstream while keeping airtight with the sample analysis chamber 12. It can be easily moved to the side seal member 3 side. However, the upstream seal member 2 may not have such a configuration. For example, in this example, 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 In a state where the film sample F is sandwiched between the ring 4b and a part of the film sample F while projecting from the sample analysis unit 10 (sample analysis chamber 12) while being hermetically sealed with the sample analysis unit 10 (sample analysis chamber 12), 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.
下流側シール部材３は、下流側Ｏリング４ｂが試料ホルダ３２から露出するフィルム試料Ｆのガス透過面と当接するよう一部が突出した状態で埋設される下流側Ｏリング保持部３’を有し、試料分析部１０の真空容器１１内壁に固定される。また、下流側シール部材３は、トランスファーロッド３１の進動により試料分析室１２内に搬入される試料ホルダ３２と下流側Ｏリング４ｂとが当接する位置に配される。したがって、下流側Ｏリング４ｂの位置調整を行うことなく、トランスファーロッド３１の進動操作を行うだけで、試料ホルダ３２に挿入されたフィルム試料Ｆと下流側Ｏリング４ｂとを当接させ、当接後、下流側シール部材３に対する上流側シール部材２の離間・接近操作を行うだけで、試料ホルダ３２を上流側Ｏリング４ａと下流側Ｏリング４ｂとで狭持させることができる。また、測定後、トランスファーロッド３１の進動先に試料ホルダ３２が存在するため、トランスファーロッド３１の進動操作を行うだけで、トランスファーロッド３１の一端側に試料ホルダ３２とを取着させることができ、トランスファーロッド３１による試料ホルダ３２の回収を容易に行うことができる。
また、本例では、下流側シール部材３は、一の面の外周側に厚肉の部として下流側Ｏリング保持部３’が形成され、中央が開口された略円盤状の部材として形成される。
なお、下流側シール部材３としては、下流側Ｏリング４ｂを除き、ステンレス鋼等の公知の金属材料で形成することができる。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 transmission 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. After the contact, 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.
Further, in this example, 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
The downstream seal member 3 can be formed of a known metal material such as stainless steel, except for the downstream O-ring 4b.
ここで、試料ホルダ３２及び上流側及び下流側Ｏリング４ａ，ｂの詳細及びこれら部材の関係について、図３（ａ），（ｂ），図４を参照しつつ説明する。なお、図３（ａ）は、試料ホルダ部を説明する説明図であり、図３（ｂ）は、図３（ａ）のＡ−Ａ線断面を示す断面図であり、図４は、Ｏリングを説明する説明図である。 Here, the details of the sample holder 32 and the upstream and downstream O-rings 4a, 4b and the relationship between these members will be described with reference to FIGS. 3 (a), 3 (b), and 4. 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, and FIG. It is explanatory drawing explaining a ring.
図３（ａ），（ｂ）に示すように、試料ホルダ３２は、中央に直径Φ１の円形開口部が形成され、ステンレス鋼等の公知の金属材料で形成される２枚の金属板３３ａ，３３ｂとの間にフィルムＦを内挿した状態でビス３４ａ〜ｄにより金属板３３ａ，３３ｂを密着させて固定可能とされ、前記開口部からフィルム試料Ｆの一面（ガス暴露面）と、反対側の他の面（ガス透過面）とが露出される。
また、試料ホルダ３２は、取付部３５が形成され、トランスファーロッド３１の一端側と取付部３５とのスイッチ式の嵌合やこれらの磁着等により、トランスファーロッド３１と脱着自在に取着可能とされる。なお、磁着等させる場合には、必ずしも、取付部３５を設ける必要はない。As shown in FIGS. 3 (a) and 3 (b), the sample holder 32 is formed with two metal plates 33a each having a circular opening having a diameter Φ1 at the center and formed of a known metal material such as stainless steel. , 33b with the metal plate 33a, 33b in close contact with the screws 34a-d with the film F inserted between them, and can be fixed, opposite the one surface (gas exposed surface) of the film sample F from 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.
一方、上流側及び下流側Ｏリング４ａ，ｂは、それぞれフッ素ゴム等の公知の樹脂材料やインジウム、金等の軟性金属材料で形成され、外径がΦ２、内径がΦ３とされる（図４参照）。
上流側及び下流側Ｏリング４ａ，ｂの外径Φ２は、試料ホルダ３２開口部の直径Φ１よりも小さく上流側及び下流側Ｏリング４ａ，ｂで、直接、試料ホルダ３２から露出する状態のフィルム試料Ｆを狭持可能とされ、内径Φ３で囲まれた領域がフィルム試料Ｆのガス透過領域とされる。また、上流側及び下流側Ｏリング４ａ，ｂとしては、非シール時における断面形状が円形状のものであってもよいが、高い気密性を得る観点から、断面形状が四角形状のものが好ましい。
なお、この例は、説明を簡単にするためのものであり、試料ホルダ３２の前記開口部は、上流側及び下流側Ｏリング４ａ，ｂの外径がΦ２よりも大きいサイズであれば、特に円形である必要はなく、また、上流側及び下流側Ｏリング４ａ，ｂは、フィルム試料Ｆを狭持可能である限り、同じ材質、全く同じ大きさである必要はない。On the other hand, 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 Φ 2 and an inner diameter of Φ 3 ( (See FIG. 4).
The outer diameter Φ 2 of the upstream and downstream O-rings 4a, 4b is smaller than the diameter Φ 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 Φ 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. .
Note that 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.
ガス透過度測定装置１００について再び図１を参照しつつ説明する。
シール機構１では、上流側Ｏリング４ａと下流側Ｏリング４ｂとでフィルム試料Ｆを狭持した状態で、フィルム試料Ｆの前記ガス暴露面と上流側Ｏリング４ａの内側と上流側シール部材２の内側とで画成されるガス暴露室４０及びフィルム試料Ｆの前記ガス透過面と下流側Ｏリング４ｂの内側と下流側シール部材３の内側と試料分析部１０（真空容器１１）の内壁で画成されるガス透過量測定室４１を形成する。The gas permeability measuring apparatus 100 will be described with reference to FIG. 1 again.
In the seal mechanism 1, 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.
また、下流側シール部材３（下流側Ｏリング保持部３’）では、下流側シール部材３から一部が突出する下流側Ｏリング４ｂの内側に一部が開口された金属板５が嵌着される等により、フィルム試料Ｆが金属板５により支持されることが好ましい。即ち、ガス暴露室４０よりもガス透過量測定室４１の方が圧力が小さいため、フィルム試料Ｆがガス透過量測定室４１側に引き寄せられ、試料フォルダ３２からの外れや湾曲により上流側及び下流側Ｏリング４ａ，ｂの内径Φ３で囲まれた領域でフィルム試料Ｆのガス透過領域を見積もれない状況が発生することがあり、フィルム試料Ｆの前記ガス透過面側を金属板５で支持することが好ましい。
なお、金属板５としては、ステンレス鋼等の公知の金属材料で形成され、任意の場所に一又は複数の開口が形成された金属板やメッシュ状に開口が形成された金属板等を用いることができる。In addition, in the downstream seal member 3 (downstream O-ring holding portion 3 ′), 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. For example, 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. 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.
In addition, as 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.
ガス透過量計測部４２（ガス分析器）は、試料分析部１０（真空容器１１）のガス透過量測定室４１を画成する部分と接続され、フィルム試料Ｆからガス透過量測定室４１内に透過したガス透過量を測定する。ガス透過量計測部４２としては、特に制限はなく、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。
また、ガス透過度の測定方法に応じて、試料分析部１０（真空容器１１）のガス透過量測定室を画成する部分と接続され、ガス透過量測定室４１内を排気する第３の真空ポンプ４３が配される。即ち、ガス透過度をガス透過量測定室４１内を真空排気しつつ、ガス透過量測定室４１内壁への気体の吸脱着反応が平衡で、かつ、ガス透過量測定室４１内でのガス透過量と真空ポンプの排気量とが平衡となった時点における圧力等を計測してガス透過度を測定する場合、その真空ポンプとして第３の真空ポンプ４３が配される。
第３の真空ポンプ４３としては、公知の真空ポンプを用いることができるが、ハイガスバリア性のフィルムを測定対象とする場合、ガス透過量測定室４１内を１０−６Ｐａ以下に排気可能なものが好ましく、例えば、ターボ分子ポンプ等を用いることができる。
試料分析室１２内を第２の真空ポンプ１３で真空排気した後、ガス透過量測定室４１を形成し、フィルム試料Ｆからのガス透過量をガス透過量測定室４１内における圧力上昇又はガス量の増加として測定する場合には、必ずしも第３の真空ポンプ４３を配する必要はない。
なお、ガス透過度測定装置１００は、試料準備部２０と試料分析部１０とを鉛直方向に連結させた例に係るが、水平方向に連結させてもよい。この場合、フィルム試料Ｆが水平面に対して垂直に配されるよう、シール機構１を構成することが好ましい。
また、ガス透過度測定装置１００は、本発明の一実施形態を示すものであり、本発明は、この実施形態に限定されない。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. There is no restriction | limiting in particular as the gas permeation | 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.
Further, 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. When the gas permeability is measured by measuring the pressure and the like at the time when the amount and the exhaust amount of the vacuum pump are in equilibrium, a third vacuum pump 43 is disposed as the vacuum pump.
As the third vacuum pump 43, a known vacuum pump can be used, but when a high gas barrier film is a measurement target, the gas permeation amount measurement chamber 41 can be evacuated to 10 −6 Pa or less. For example, 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 set to the pressure increase or 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.
In addition, although 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.
Moreover, the gas permeability measuring apparatus 100 shows one embodiment of the present invention, and the present invention is not limited to this embodiment.
次に、ガス透過度測定装置１００の動作について図１を参照しつつ説明をする。
ゲート弁３０を閉じた状態で、試料分析室１２内を第２の真空ポンプ１３で排気する。ガス透過度測定対象のフィルム試料Ｆがハイバリア性（ガス透過度が高い）のフィルムである場合、試料分析室１２内を１０−３Ｐａ以下程度に真空排気する。Next, the operation of the gas permeability measuring apparatus 100 will be described with reference to FIG.
With the gate valve 30 closed, the sample analysis chamber 12 is evacuated by the second vacuum pump 13. When the film sample F to be measured for gas permeability is a high barrier (high gas permeability) film, the sample analysis chamber 12 is evacuated to about 10 −3 Pa or less.
また、真空容器２１の密閉扉（不図示）を通じて挿通部２６から真空容器２１内に垂下されたトランスファーロッド３１の一端側に試料ホルダ３２を取着させる。なお、トランスファーロッド３１からの試料ホルダ３２の着脱は、例えば、トランスファーロッド３１の電磁石で試料ホルダ３２が取着される場合、前記電磁石の励磁をオンオフ動作させて行う。トランスファーロッド３１に取着される試料ホルダ３２は、試料ホルダストック機構２５におけるストック部２３にストックされていないものを直接取着させて用いてもよいが、吸着ガス等を脱離させる観点から、予めストック部２３にストックさせておいたものが好ましい。試料ホルダストック機構２５のストック部２３に対する試料ホルダ３２のストックは、真空容器２１の密閉扉（不図示）を通じて行う。密閉扉は、作業完了後、速やかに閉じるようにする。
また、試料準備室２７内に滞留される試料ホルダ３２等に吸着される水蒸気等は、ヒータ２２による加熱により脱離され、第１の真空ポンプ２８で効率的に排気可能とされる。ヒータ２２による加熱は、フィルム試料Ｆの耐熱温度未満の温度で行う。また、第１の真空ポンプ２８では、フィルム試料Ｆがハイバリア性のフィルムである場合、試料準備室２７内を１０−３Ｐａ以下程度に真空排気させる。In addition, 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.
Further, 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. Further, in the first vacuum pump 28, when the film sample F is a high barrier film, the inside of the sample preparation chamber 27 is evacuated to about 10 −3 Pa or less.
試料分析部１０では、予め上流側シール部材２のガス導入部２ｂの真空容器１１外に突出して延在する部分又は当該部分と接続される配管をスライド操作し、上流側Ｏリング４ａと下流側Ｏリング４ｂとの間に試料ホルダ３２を挿通させるよう上流側シール部材２（上流側Ｏリング保持部２ａ）を下流側シール部材３（下流側Ｏリング保持部３’）から離間させておく。
ストック部２３にストックされた試料ホルダ３２をトランスファーロッド３１に取着させた後、ゲート弁３０を開き、トランスファーロッド３１を試料分析部１２内の所定の深さまで搬送操作することで、試料ホルダ３２を内挿される試料フィルムＦの上流側Ｏリング４ａと下流側Ｏリング４ｂとによる狭持位置まで搬送する。
この状態で、上流側シール部材２のスライド操作により、上流側Ｏリング保持部２ａを下流側Ｏリング保持部３に接近させて上流側Ｏリング４ａと下流側Ｏリング４ｂとでフィルム試料Ｆを狭持させる。
この時、シール機構１内では、フィルム試料Ｆの前記ガス暴露面（一の面）と上流側Ｏリング４ａの内側と上流側シール部材２の内側とで画成されるガス暴露室４０と、フィルム試料Ｆの前記ガス透過面（一の面と反対側の他の面）と下流側Ｏリング４ｂの内側と下流側シール部材３の内側と試料分析部１０（真空容器１１）の内壁で画成されるガス透過量測定室４１とが気密状態で形成される。
その後、試料ホルダ３２からトランスファーロッド３１を脱着させ、トランスファーロッド３１を試料準備室２７に戻し、ゲート弁３０を再び閉じ、引き続き第２の真空ポンプ１３で試料分析室１２内を真空排気し、ガス透過度測定の測定準備を完了させる。In the sample analysis unit 10, 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.
After the sample holder 32 stocked in the stock unit 23 is attached to the transfer rod 31, the gate valve 30 is opened, and the transfer rod 31 is transported to a predetermined depth in the sample analysis unit 12. Is transported to a holding position by the upstream O-ring 4a and the downstream O-ring 4b of the sample film F to be inserted.
In this state, the upstream O-ring holding portion 2a is moved closer to the downstream O-ring holding portion 3 by the sliding operation of the upstream sealing member 2, and the film sample F is moved between the upstream O-ring 4a and the downstream O-ring 4b. Hold it.
At this time, in the seal mechanism 1, 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.
Thereafter, 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.
本例におけるガス透過度測定では、ガス透過量測定室４１内を第３の真空ポンプで真空排気しつつ、上流側シール部材２のガス導入部２ｂを介してガス供給源６から供給される測定用ガスをガス暴露室４０内に導入させ、フィルム試料Ｆからガス透過量測定室４１内に透過する前記測定用ガスの透過量を透過量ガス透過量計測部４２（ガス分析器）で計測して行う。計測は、ガス透過量測定室４１内壁への気体の吸脱着反応が平衡で、かつ、ガス透過量測定室４１内でのガス透過量と第３の真空ポンプ４３の排気量とが平衡となった時点における圧力等を計測してガス透過度を測定する。なお、フィルム試料Ｆがハイバリア性のフィルムである場合、ガス透過量測定室４１内を第３の真空ポンプを用いて１０−６Ｐａ以下程度に真空排気する。In the gas permeability measurement in this example, 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. In the measurement, 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. When 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.
次に、本発明の効果について、ガス透過度測定装置１００を例にとり詳細に説明する。
ガス透過度測定装置１００では、装置に対してフィルム試料Ｆを搬出入する度に装置内を大気に暴露することがなく、予め所望の真空環境にまで真空排気された試料分析部１０でガス透過度を測定するため、短時間で測定条件の真空環境を得ることができ、延いては、フィルム試料Ｆのガス透過度を短時間で効率的に測定することができる。
また、フィルム試料Ｆ、試料ホルダ３２等に吸着したガスをガス透過度測定前に予め試料準備部２０で排除することができるため、試料分析部１０において、これらが脱離せず短時間で測定条件の真空環境を得ることができ、延いては、フィルム試料Ｆのガス透過度を短時間で効率的に測定することができる。
また、試料準備部２０において、試料ホルダストック機構２５に試料ホルダ３２をストックしておくことで、試料ホルダ３２に吸着したガス、水蒸気等が排除された試料ホルダ３２を予め準備することができる。したがって、試料分析部１０においてより短時間で測定条件の真空環境を得ることができ、延いては、フィルム試料Ｆのガス透過度を短時間で効率的に測定することができる。Next, the effect of the present invention will be described in detail by taking the gas permeability measuring apparatus 100 as an example.
In the gas permeability measuring apparatus 100, 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. In order to measure the degree, 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. 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. Thus, the gas permeability of the film sample F can be measured efficiently in a short time.
In addition, by storing 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.
また、ガス透過度測定装置１００では、装置内に配され、また、金属製の試料ホルダ３２の開口部直径Φ１よりも小さな外径Φ２の上流側及び下流側Ｏリング４ａ，ｂで直接試料ホルダ３２を狭持してガス透過度測定を行うため、高精度にガス透過度の測定を行うことができ、延いては、１０−６ｇ／ｍ２／ｄａｙといったハイバリア性のフィルム試料を測定対象とすることができる。
この点について、更に、図２，図５〜７を参照しつつ、下記参考例１及び２に係るガス透過度測定装置と比較した説明を行う。なお、図５は、参考例１に係るガス透過度測定装置のシール機構を拡大して示す説明図であり、図６は、参考例１に係るガス透過度測定装置の変形例に係るガス透過度測定装置のシール機構を拡大して示す説明図であり、図７は、参考例２に係るガス透過度測定装置シール機構を拡大して示す説明図である。Further, in the gas permeability measuring apparatus 100, the upstream and downstream O-rings 4a and 4b having an outer diameter Φ 2 smaller than the opening diameter Φ 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 precision. As a result, a high barrier film sample such as 10 −6 g / m 2 / day can be obtained. It can be a measurement object.
With respect to this point, a description will be given in comparison with the gas permeability measuring apparatus according to Reference Examples 1 and 2 below, with reference to FIGS. 2 and 5 to 7. 5 is an explanatory diagram showing an enlarged seal mechanism of the gas permeability measuring device according to Reference Example 1, and 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.
参考例１に係るガス透過度測定装置では、図５に示すように、上流側及び下流側Ｏリング４ａ，ｂの外径Φ２に対して、開口部の直径Φ１が小さい金属製の試料ホルダ５０を用いることとし、試料ホルダ５０の金属板５１ａ，５１ｂでフィルム試料Ｆを狭持してガス透過度測定を行う点で、ガス透過度測定装置１００と異なる。なお、符号５３は、トランスファーロッド３１への取付部を示す。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.
この参考例１に係るガス透過度測定装置をガス透過度測定を行うと、ガス導入部２ｂから導入される測定用ガスが、Ｏリングによるシールがないため金属板５１ａとフィルム試料Ｆとの間から試料分析室１２内に漏れ出した後、金属板５１ｂとフィルム試料Ｆとの間からガス透過量測定室側に漏れ出し（図５中の黒矢印参照）、フィルム試料Ｆを透過したガス（図５中の白抜き矢印参照）と混ざり込み、フィルム試料Ｆのガス透過度測定を精度良く実施することができない。 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.
また、図６に示すように、参考例１に係るガス透過度測定装置の問題を解消する変形例として、金属板５１ａ，５１ｂの対向面にＯリング５２ａ，ｂを埋設し、これらＯリング５２ａ，ｂでフィルム試料Ｆを狭持させても、Ｏリング５２ａ，ｂが試料ホルダ５０とともに装置内外に搬出入されるため、装置外でＯリング５２ｂに吸収されたガスが金属板５１ｂとフィルム試料Ｆとの間からガス透過量測定室側に漏れ出し（図６中の黒矢印参照）、フィルム試料を透過したガス（図６中の白抜き矢印参照）と混ざり込み、フィルム試料Ｆのガス透過度測定を精度良く実施することができない。 Moreover, as shown in FIG. 6, as a modification to solve the problem of the gas permeability measuring apparatus according to Reference Example 1, 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.
参考例２に係るガス透過度測定装置では、図７に示すように、上流側及び下流側Ｏリング４ａ，ｂの外径Φ２に対して、開口部の直径Φ１が小さい金属製の試料ホルダ６０を用いることとし、試料ホルダ６０の金属板６１ａ，６１ｂでフィルム試料Ｆを狭持してガス透過度測定を行う点で、ガス透過度測定装置１００と異なる。また、金属板５１ａよりもサイズが小さい金属板６１ａを用い、金属板６１ｂのみを上流側及び下流側Ｏリング４ａ，ｂで狭持する点で、参考例１に係るガス透過度測定装置と異なる。なお、符号６３は、トランスファーロッド３１への取付部を示す。In the gas permeability measuring apparatus according to Reference Example 2, as shown in FIG. 7, a metal sample in which the diameter Φ 1 of the opening is smaller than the outer diameter Φ 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.
この参考例２に係るガス透過度測定装置では、参考例１に係るガス透過度測定装置と異なり、前記測定用ガスが試料分析室１２内に漏れ出すことはないものの、前記測定用ガスが金属板６１ｂとフィルム試料Ｆとの接合面に直接到達し、この接合面には、Ｏリングによるシールがされていないことから、前記測定用ガスが金属板６１ｂとフィルム試料Ｆとの間からガス透過量測定室側に漏れ出し（図７中の黒矢印参照）、フィルム試料を透過したガス（図７中の白抜き矢印参照）と混ざり込み、ガス透過度測定を正確に実施することができない。また、金属板６１ｂとフィルム試料Ｆとの接合面にＯリングを配しても、参考例１に係るガス透過度測定装置の変形例について説明した問題が生じ、フィルム試料Ｆのガス透過度測定を精度良く実施することができない。 Unlike the gas permeability measuring apparatus according to Reference Example 1, 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. In addition, even when an O-ring is provided on the joint surface between the metal plate 61b and the film sample F, the problem described in the modification of the gas permeability measuring device according to Reference Example 1 occurs, and the gas permeability measurement of the film sample F occurs. Cannot be carried out with high accuracy.
これらに対し、ガス透過度測定装置１００では、前記測定ガスのガス透過量測定室側に漏れ出しがなく、フィルム試料Ｆを透過したガスのみを測定対象とすることができ（図２中の白抜き矢印参照）、フィルム試料Ｆのガス透過度測定を高精度に実施することができる。 On the other hand, in 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.
１ シール機構
２ 上流側シール部材
２ａ 上流側Ｏリング保持部
２ｂ ガス導入部
３ 下流側シール部材
３’ 下流側Ｏリング保持部
４ａ，ｂ，５２ａ，ｂ Ｏリング
５ 金属板
６ ガス供給源
１０ 試料分析部
１１，２１ 真空容器
１２ 試料分析室
１３ 第２の真空ポンプ
１４ 試料ホルダ支持部
２０ 試料準備部
２２ ヒータ
２３ ストック部
２４ ストック部支持部
２５ 試料ホルダストック機構
２６ 挿通部
２７ 試料準備室
２８ 第１の真空ポンプ
３０ ゲート弁
３１ トランスファーロッド
３２，５０，６０ 試料ホルダ
３３ａ，ｂ，５１ａ，ｂ，６１ａ，ｂ 金属板
３４ａ〜ｄ ビス
３５，５３，６３ 取付部
４０ ガス暴露室
４１ ガス透過量測定室
４２ ガス透過量計測部（ガス分析器）
４３ 第３の真空ポンプ
１００ ガス透過度測定装置DESCRIPTION OF SYMBOLS 1 Seal mechanism 2 Upstream side seal member 2a Upstream side O-ring holding | maintenance part 2b Gas introduction part 3 Downstream side sealing member 3 'Downstream side O-ring holding | maintenance part 4a, b, 52a, b O-ring 5 Metal plate 6 Gas supply source 10 Sample Analysis unit 11, 21 Vacuum container 12 Sample analysis chamber 13 Second vacuum pump 14 Sample holder support unit 20 Sample preparation unit 22 Heater 23 Stock unit 24 Stock unit support unit 25 Sample holder stock mechanism 26 Insertion unit 27 Sample preparation chamber 28 1 Vacuum pump 30 Gate valve 31 Transfer rod 32, 50, 60 Sample holder 33a, b, 51a, b, 61a, b Metal plate 34a to d Screw 35, 53, 63 Mounting portion 40 Gas exposure chamber 41 Gas permeation amount measurement Chamber 42 Gas permeation measurement unit (gas analyzer)
43 3rd vacuum pump 100 Gas permeability measuring device
Claims (6)
一端側が前記試料ホルダと脱着自在に取着可能とされるトランスファーロッドと、
前記トランスファーロッドを内部空間に気密状態で進退動自在として挿通させる挿通部が形成されるとともに前記試料ホルダが前記内部空間に滞留可能とされる試料準備部と、前記トランスファーロッドの進退動により内部空間で前記試料ホルダが搬出入可能とされる試料分析部と、開状態で前記試料準備部内−前記試料分析部内間で前記試料ホルダが搬出入可能とされ、閉状態で前記試料準備部内−前記試料分析部内間を気密状態で密閉可能とされるゲート弁とを有する真空容器部と、
下流側Ｏリングが前記試料ホルダから露出する前記フィルム試料の前記ガス透過面と当接するよう一部が突出した状態で埋設される下流側Ｏリング保持部を有し、前記試料分析部の内壁に固定される下流側シール部材と、上流側Ｏリングが前記試料ホルダから露出する前記フィルム試料の前記ガス暴露面と当接するよう一部が突出した状態で埋設され、前記上流側Ｏリングと前記下流側Ｏリングとで前記試料ホルダから露出する前記フィルム試料を狭持可能に前記下流側Ｏリング保持部と対向配置される上流側Ｏリング保持部及びガス供給源と接続されるガス導入部が形成され、前記下流側Ｏリング保持部に接近させて前記上流側Ｏリングと前記下流側Ｏリングとで前記フィルム試料を狭持させ、前記下流側Ｏリング保持部から離間させて前記上流側Ｏリングと前記下流側Ｏリングとの間に前記試料ホルダを挿通させるように少なくとも前記上流側Ｏリング保持部を移動可能として前記試料分析部に支持される上流側シール部材とで構成され、前記上流側Ｏリングと前記下流側Ｏリングとで前記フィルム試料を狭持した状態で、前記フィルム試料の前記ガス暴露面と前記上流側Ｏリングの内側と前記上流側シール部材の内側とで画成されるガス暴露室及び前記フィルム試料の前記ガス透過面と前記下流側Ｏリングの内側と前記下流側シール部材の内側と前記試料分析部の内壁で画成されるガス透過量測定室を形成するシール機構と、
前記試料準備部と接続され、前記真空容器内を排気する第１の真空ポンプと、
前記試料分析部の前記下流側Ｏリングからみて前記下流側シール部材の外側の位置に接続され、前記真空容器内を排気する第２の真空ポンプと、
前記試料分析部の前記ガス透過量測定室を画成する部分と接続され、前記フィルム試料から前記ガス透過量測定室内に透過した測定用ガスの透過量を測定するガス透過量計測器と、
を備えることを特徴とするガス透過度測定装置。A metal sample holder in which an opening is formed, and the film sample is removably inserted in a state where both the gas exposed surface and the gas permeable surface of the film sample are exposed from the opening,
A transfer rod whose one end is detachably attached to the sample holder;
An insertion part for allowing the transfer rod to be inserted into the internal space in an airtight state so as to be movable forward and backward is formed, and a sample preparation part for allowing the sample holder to stay in the internal space; and an internal space by the forward and backward movement of the transfer rod The sample holder can be carried in and out, and the sample holder can be carried in and out between the sample preparation unit and the sample analysis unit in the open state, and in the sample preparation unit and the sample in the closed state. A vacuum vessel portion having a gate valve that can be hermetically sealed between the analysis portions;
A downstream O-ring holding portion embedded in a protruding state so that the downstream O-ring is in contact with the gas permeable surface of the film sample exposed from the sample holder, and is provided on the inner wall of the sample analysis portion A downstream seal member to be fixed and an upstream O-ring are embedded with a part protruding so as to come into contact with the gas exposure surface of the film sample exposed from the sample holder, and the upstream O-ring and the downstream O-ring A gas inlet that is connected to a gas supply source and an upstream O-ring holding portion that is disposed opposite to the downstream O-ring holding portion are formed so that the film sample exposed from the sample holder can be held by the side O-ring. The film sample is sandwiched between the upstream O-ring and the downstream O-ring by being brought close to the downstream O-ring holding portion and separated from the downstream O-ring holding portion. The upstream O-ring holding member is supported by the sample analysis unit so that at least the upstream O-ring holding unit can be moved so that the sample holder is inserted between the upstream O-ring and the downstream O-ring. In the state where the film sample is held 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 A gas exposure chamber defined by the gas exposure chamber defined, the gas permeable 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 sealing mechanism to be formed;
A first vacuum pump connected to the sample preparation unit and evacuating the vacuum vessel;
A second vacuum pump connected to a position outside the downstream seal member as viewed from the downstream O-ring of the sample analyzer and exhausting the vacuum vessel;
A gas permeation amount measuring device connected to a portion defining the gas permeation amount measurement chamber of the sample analysis unit and measuring a permeation amount of a measurement gas permeated from the film sample into the gas permeation amount measurement chamber;
A gas permeability measuring device comprising:
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102515087B1 (en) * | 2022-12-06 | 2023-03-29 | 한국건설기술연구원 | Test apparatus for measuring air permeability coefficient of concrete specimen, and test method using the same |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6446683B2 (en) * | 2015-03-05 | 2019-01-09 | 埼玉県 | Water vapor permeability measuring device and water vapor permeability measuring method of sample |
| WO2018155678A1 (en) * | 2017-02-27 | 2018-08-30 | 国立研究開発法人産業技術総合研究所 | Device for evaluating gas barrier properties and method for evaluating gas barrier properties |
| KR102538826B1 (en) * | 2018-11-12 | 2023-06-02 | 삼성디스플레이 주식회사 | Moisture permeability measuring device |
| CN109813643B (en) * | 2019-01-01 | 2021-06-08 | 中国人民解放军63653部队 | Concrete and gas permeability measuring method of surface coating material thereof |
| DE102020209493A1 (en) * | 2020-07-28 | 2022-02-03 | Robert Bosch Gesellschaft mit beschränkter Haftung | Apparatus and method for determining a gas permeation index of a layer of material |
| KR102632280B1 (en) * | 2023-04-28 | 2024-02-02 | 한국표준과학연구원 | Sample Holder with Double Sealing and Exhaust Structure |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0441324Y2 (en) * | 1984-10-15 | 1992-09-29 | ||
| JPS63157870A (en) * | 1986-12-19 | 1988-06-30 | Anelva Corp | Substrate treatment device |
| JP3264458B2 (en) * | 1993-02-17 | 2002-03-11 | 三井化学株式会社 | Gas permeability measuring device for film |
| JP2007147648A (en) * | 2000-12-01 | 2007-06-14 | Ebara Corp | Defect inspection method and substrate inspection device |
| JP3930871B2 (en) * | 2004-06-04 | 2007-06-13 | 株式会社クリエテック | Moisture permeability / gas permeability measuring device and gas permeability measuring method |
| GB2437136A (en) * | 2006-03-30 | 2007-10-17 | Ltd Technolox | Measuring rate of permeation |
| CN101809427B (en) * | 2007-09-28 | 2013-09-04 | 株式会社爱发科 | Device for measuring steam permeability, and method for the device |
| US8388742B2 (en) * | 2010-01-13 | 2013-03-05 | E I Du Pont De Nemours And Company | Apparatus to measure permeation of a gas through a membrane |
| JP5734109B2 (en) * | 2011-06-20 | 2015-06-10 | 株式会社住化分析センター | Measuring apparatus and measuring method |
| JP2014002038A (en) * | 2012-06-19 | 2014-01-09 | Seinan Kogyo Kk | Vapor permeability measuring apparatus and vapor permeability measuring method |
| JP6345421B2 (en) * | 2013-01-31 | 2018-06-20 | 国立研究開発法人産業技術総合研究所 | Gas barrier property evaluation apparatus and evaluation method |
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2015
- 2015-11-24 WO PCT/JP2015/082853 patent/WO2016114003A1/en active Application Filing
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|---|---|---|---|---|
| KR102515087B1 (en) * | 2022-12-06 | 2023-03-29 | 한국건설기술연구원 | Test apparatus for measuring air permeability coefficient of concrete specimen, and test method using the same |
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| JPWO2016114003A1 (en) | 2017-07-27 |
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