JP3106379U - Multi-cell transmission measurement device - Google Patents

Abstract

A multi-cell permeation amount measuring apparatus is provided in which a plurality of cell units are arranged while saving a plane space, and each cell unit can be easily adjusted and maintained.
A cell assembly 3 includes a plurality of cell assemblies 3, a vacuum manifold (26) having a plurality of vacuum connection ports 27, and a control device. The cell assembly 3 sandwiches a film to be tested for measuring the amount of permeation therebetween. A cell unit 9 comprising a cell 11 and a lower cell 14, a conducting tube 15 extending downward from the lower surface of the lower cell, a first on-off valve 16, a pressure sensor 17, The on-off valve 18 and the vacuum joint 28 are connected to the vacuum connection port 27 in a detachable manner, and the controller opens and closes the first on-off valve 16 and the second on-off valve 18. Is a multi-cell permeation amount measuring apparatus for controlling
[Selection] Figure 1

Description

  The present invention relates to a thin film permeation measuring apparatus for measuring a permeation amount of a gas or liquid that permeates a film or the like, and includes a plurality of measurement cells and capable of simultaneously measuring a permeation amount of a plurality of test films. It is about.

The differential pressure method is employed as a method for measuring the permeability of gases and liquids such as plastic films. In the differential pressure method, a membrane to be tested is sandwiched between an upper cell equipped with a test gas inlet and a lower cell connected to a pressure detector, and the amount of test gas that has permeated the membrane to be tested is detected by pressure change. (For example, refer nonpatent literature 1).
2. Description of the Related Art A permeation amount measuring apparatus that performs measurement by a differential pressure method is known. This apparatus usually includes a single measurement cell (see, for example, Patent Document 1).
Registered Utility Model No. 3096609 JIS K 7126 Gas permeability test method for plastic films and sheets

  In the measurement of the transmittance by the differential pressure method, the amount of permeation is measured after the time when the amount of permeation becomes constant (at the time of stabilization). The time required for stabilization depends on the permeability and other characteristics of the membrane to be tested, but membranes with lower permeability require longer time for stabilization, and there are membranes to be tested that require several weeks for stabilization. is there. Accordingly, it is desirable to increase the number of measurement cells when measuring a large number of films to be tested.

However, it is necessary to prepare a large number of permeation amount measuring apparatuses having a single measuring cell, and a large space is required, and the cost increases. On the other hand, if the number of measurement cells included in a single permeation amount measuring device is increased, test gas piping and vacuum piping become complicated.
In addition, the differential pressure method tends to cause a problem that the degree of vacuum is not stable due to a gas leak from the permeate-side piping and parts. In addition, a liquid such as an organic solvent may be used instead of the test gas as the permeator.If the film under test breaks during measurement, the liquid enters the path in the permeate-side piping and parts, and cleaning is performed. Necessary. In such a case, it is necessary to remove the specific one measurement cell system and perform adjustment and cleaning.
Furthermore, it is necessary to arrange a plurality of measurement cells in a compact manner.

  In order to solve the above problems, the multi-cell transmission amount measuring device of the present invention is composed of a plurality of cell assemblies, a vacuum manifold having a plurality of vacuum connection ports, and a control device, and the cell assembly measures the transmission amount. A cell unit composed of an upper cell and a lower cell sandwiching a film to be tested, a conducting tube extending downward from the lower surface of the lower cell, and a first opening / closing array connected downward to the other end of the conducting tube in order A valve, a pressure sensor, a second on-off valve, and a vacuum joint, the vacuum joint is detachably connected to the vacuum connection port, and the control device opens and closes the first on-off valve and the second on-off valve. Is a multi-cell permeation amount measuring apparatus for controlling

  Since the cell assembly composed of the cell unit, the conducting pipe, the on-off valve, etc. is arranged in the vertical direction in this order, the entire cell assembly is arranged in the vertical direction. I can do it. In addition, since the connecting portion with the vacuum manifold is detachably connected, the single cell assembly can be easily detached.

In the present invention, the number of the plurality of cell assemblies is not particularly limited as long as it is 2 or more, but the number is preferably 5 or more and 100 or less, and more preferably 10 or more, in order to achieve the features of the present invention better. 100 or less.
“Arranged in the downward direction” not only means that the first on-off valve, pressure gauge, and second on-off valve are arranged with their centers aligned in the vertical direction, but their centers do not necessarily coincide with the vertical direction. , Alternately arranged up and down, the first on-off valve, the connection part of the pressure gauge, and the second on-off valve are arranged vertically (that is, the connection pipe of the pressure gauge is bent, the pressure The main body portion of the meter includes an arrangement positioned above or below either of the first and second on-off valves.

A gas introduction joint may be provided in the upper cell, and a gas outlet joint may be provided in addition to the gas introduction joint. In addition, a plurality of the gas inlet joints and / or gas outlet joints may be provided in a single upper cell. The gas inlet fitting is usually connected to the test gas supply via a conduit. When the test gas is a gas (for example, oxygen, carbon dioxide, etc.) at normal temperature and pressure, the test gas supply is usually a constant volume chamber. When the test gas is a liquid at normal temperature and pressure (for example, an organic solvent (ethanol, methanol, etc.), water vapor, etc.), the test gas supply is usually a chamber having a constant volume liquid reservoir and an upper space. .
Furthermore, the upper cell may have a liquid reservoir. That is, when the test gas is liquid at normal temperature and pressure, the liquid may be held in the liquid reservoir, and the test gas may be generated in the upper cell to perform measurement.

  The first on-off valve and the second on-off valve of the plurality of cell assemblies are preferably controlled independently for each single cell assembly. However, the plurality of cell assemblies are divided into an appropriate number of sub-cell assembly groups, and the first on-off valve group and the second on-off valve group are simultaneously opened and closed for each of the plurality of cell assemblies belonging to the sub-cell assembly group. It may be performed in conjunction.

In a preferred embodiment of the present invention, the multi-cell permeation amount measuring apparatus has a gas supply manifold having a plurality of gas supply connection ports, a gas discharge manifold having a plurality of gas discharge connection ports, and the upper part. The cell may have a gas inlet joint and a gas outlet joint, the gas inlet joint may be detachably connected to the gas supply connection port, and the gas outlet joint may be detachably connected to the gas discharge connection port.
According to the present embodiment, in particular, when the test gas is a gas at normal temperature and normal pressure, the multi-cell permeation amount measuring apparatus with better operability is obtained.

  In a preferred embodiment of the present invention, the multi-cell permeation amount measuring device is a base on which the plurality of cell assemblies are disposed, the vacuum manifold is disposed in an upper space of the vacuum manifold. It has a substrate arranged in a horizontal direction, the substrate is provided with a main slit that opens at one edge of the substrate and through which the conducting pipe can pass, branches from the main slit, and the conducting pipe can pass through. A plurality of branch trunk slits are provided, and through the branch pipe slit of the cell assembly to the main trunk slit from the opening portion, the branch pipe slit is passed to the tip of the branch trunk slit to send the conductive pipe to the position. A cell assembly is arranged, the cell unit has a cylindrical shape, and the end portions of the branch stem slits are equal to or larger than the diameter of the cell unit. A plurality of the plurality of branch stem slits on a base having a substrate disposed at a distance equal to or greater than a diameter of the cell unit from a center line of the main trunk slit; In the state where the plurality of cell assemblies are further disposed, the individual cell assemblies in the plurality of cell assemblies are brought into contact with the plurality of remaining cell assemblies without contacting the branch cell assemblies. The plurality of cell assemblies may be arranged so as to pass through the slit and the main slit and be removed from one edge of the substrate.

The permeation amount measuring cell unit is heavy, and in order to support a plurality of cell units by a single substrate, it is preferable that the substrate is as continuous as possible with few cut portions. The substrate according to this embodiment provided with slits is suitable for supporting such a plurality of cell units.
In addition, even if a plurality of cell assemblies are arranged, it becomes possible to remove one specific cell assembly without moving the remaining cell assemblies from the arrangement state, and it is suitable for adjustment and maintenance. .

In another preferred embodiment of the present invention, the vacuum manifold has n vacuum connection ports (n is a positive integer of 2 or more and 10 or less), and is provided with an on-off valve at a branch point. It may be branched to a vacuum manifold.
According to this embodiment, in the case where a failure such as a vacuum holding state occurs in one cell assembly, there is an advantage that the influence of the failure stops only in the cell assembly group connected to the one sub vacuum manifold. . In addition, there is an effect that it becomes easy to find a cell assembly in which a problem occurs (it is possible to omit the trouble of checking all cell assemblies).

In still another preferred embodiment of the present invention, the cell unit may have temperature control means.
In general, since a thin film has a characteristic that the amount of permeation varies depending on the temperature, it is necessary to perform measurement while keeping the temperature of the transmission cell unit constant. In order to perform measurement by changing the temperature of the cell unit, it is necessary to wait for the cell unit temperature to stabilize in addition to the permeation amount stabilization, and a long time is required until measurement. Therefore, in the present embodiment in which the temperature adjusting means is provided in the plurality of cell units, there is an effect that the advantage of the plurality of cell permeation amount measuring device is further enhanced.

  According to the present invention, it is possible to obtain a multi-cell permeation amount measuring apparatus in which a plurality of cell units are arranged while saving a plane space, and each of the cell units can be easily adjusted and maintained.

  The multi-cell transmission amount measuring apparatus according to the present invention will be further described below with reference to the drawings. The dimensions, materials, shapes, relative positions, etc. of members and parts described in the embodiments of the present invention are not intended to limit the scope of the present invention to those unless otherwise specified. It is merely an illustrative example.

FIG. 1 is a partial cross-sectional explanatory view of a multi-cell permeation amount measuring apparatus, FIG. 2 is a surface explanatory view, and FIG. 3 is a perspective explanatory view of a base.
FIG. 1 shows five cell assemblies 3 arranged and connected in a multi-cell transmission amount measuring apparatus. The cell unit 9 includes an upper cell 11 and a lower cell 14 for supplying a test gas, and a film to be tested is sandwiched between the upper cell 11 and the lower cell 14. The upper cell 11 has a gas inlet joint 12 and a gas outlet joint 13, and the test gas is introduced into the upper cell from the gas inlet joint 12 and discharged from the gas outlet joint 13.

  Referring to FIG. 2, the gas supply manifold 21 has a plurality of gas supply connection ports 22, and each is connected to an individual gas introduction joint 12. The gas discharge manifold 23 has a plurality of gas discharge connection ports 24, each connected to an individual gas discharge joint 13. The gas supply connection port 22 and the gas discharge connection port 24 are, for example, SUS304 tubes having an outer diameter of 1.5 mm. The gas introduction joint 12 and the gas discharge joint 13 are screw holes. The bush screw is passed through the tube, and the bush screw is attached to the screw hole so as to be detachable. The other end of the gas supply manifold 21 is connected to a test gas supplier (not shown). In FIG. 2, the gas exhaust manifold connected to the upper ten cell units 9 is not shown.

In FIG. 1, 20 is a temperature controller. The lower cell 14 incorporates a heater and a temperature sensor, which are connected to the temperature controller 20 and can keep the cell unit at a constant temperature. The temperature controller 20 is connected to a bus line 32 via a connection line 37, and the bus line 32 is connected to a control device (not shown). Thereby, the temperature of each cell unit 9 can be controlled from a control device (for example, a computer). The heater and the temperature sensor built in the lower cell 14 need only have a function of keeping the cell at a constant temperature, may contain an electronic cooling element (for example, a Peltier element), and have a structure for circulating temperature-controlled water. It may be.
Further, in order to reduce heat exchange between the lower cell 14 and the substrate 5, a base portion may be provided on the lower cell 14 and / or the substrate 5 to reduce the contact area between the lower cell 14 and the substrate 5.

FIG. 4 is an explanatory perspective view of the cell assembly 3.
Referring to FIGS. 1 and 4, a conducting tube 15 opens downward in the center of the lower surface of the lower cell 14, and a first opening / closing valve 16, which is an electromagnetic valve, is attached to the lower side of the tip. A joint 29 is attached to the lower side of the first on-off valve 16 via a pipe, and a pressure sensor 17 is attached to the side of the joint 29 via a pipe. Further, a second on-off valve 18 as an electromagnetic valve is attached below the joint 29, and a vacuum joint 28 is attached below the second on-off valve 18.

  The first on-off valve 16 opens and closes the conduction between the conducting pipe 15 and the joint 29. The second on-off valve 18 opens and closes the connection between the joint 29 and the vacuum joint 28.

The first on-off valve 16 and the second on-off valve 18 are only required to be able to be remotely operated, and may be, for example, an air driven valve driven by compressed air or a hydraulically driven valve.
The pressure sensor 17 can be a pressure sensor capable of measuring pressure over time, such as a vacuum gauge using a piezoelectric element, a diaphragm type electronic sensor, a vacuum gauge using a change in heat conduction, and the like.

  The vacuum joint 28 is detachably connected to the vacuum connection port 27. The sub vacuum manifold 26 has a plurality of vacuum connection ports 27. The vacuum connection port 27 has a cylindrical shape protruding upward, and a screw is screwed on the outer periphery. The vacuum joint 28 is a flexible tube made of SUS304 having an outer diameter of 9 mm. By inserting a cap nut into the vacuum joint 28 and screwing the cap nut to the vacuum connection port 27, the vacuum connection port 27 and the vacuum joint 28 are detachably connected.

The cell unit 9, the conducting pipe 15, the first on-off valve 16, the pressure sensor 17, the second on-off valve 18, and the vacuum joint 28 constitute the cell assembly 3.
The diameter of the cell unit used in this example is 110 mm, and the size of the pressure sensor body is a cylindrical shape with a diameter of 65 mm and a height of 60 mm. The pressure sensor protrudes outward from the joint 29 by a maximum of 160 mm.

  Referring to FIG. 1, one end of sub-vacuum manifold 26 is connected to a vacuum pump (not shown) via open / close valve 41 and vacuum manifold. The vacuum pump is a pump capable of exhausting the gas in the pipe from the lower cell 14 to the vacuum manifold to a pressure of about 0.00X KPs, and a turbo molecular pump, an oil rotary pump, or the like can be used.

The first on-off valve 16, the pressure sensor 17, and the second on-off valve 18 are connected to the bus line 31 through connection lines 34, 35, and 36, respectively, and the bus line 31 is connected to the control device described above. Therefore, the control device can independently control the opening and closing of all the first on-off valves 16 and the second on-off valves 18, and also monitors the measured value of the pressure sensor 17 and further transmits the test piece from the measured value. The amount can be calculated. In order to monitor a plurality of on-off valves and pressure sensor measurement values with a single control device, for example, software may be used to perform the time sharing method. Further, it may be performed by interposing a hardware switching circuit.
The connection lines 34, 35, 36 and the bus line 31 and the connection line 37 and the bus line 32 are preferably detachably connected using plugs and sockets.

Referring to FIG. 3, the base 4 has a shape obtained by removing one side plate of a rectangular parallelepiped, and is made of iron. In the substrate 5, a main trunk slit 6 and a branch main slit 7 branched from the main slit 6 are formed. The main slit 6 opens at one edge 10 of the substrate 5. The widths of the main trunk slit 6 and the branch trunk slit 7 are determined such that the conducting tube 15 of the cell assembly 3 can pass through.
Referring to FIG. 2, the tip 51 of one branch trunk slit is provided at a distance equal to or larger than the diameter of the cell unit from the tips 52 and 53 of adjacent branch trunk slits. Furthermore, the tip 51 of the branch trunk slit is provided at a distance of at least twice the diameter of the cell unit from the tip 54 of the branch trunk slit on the opposite side across the main trunk slit 6. That is, the distal end portion of the branch trunk slit is arranged at a distance greater than the diameter of the cell unit from the center line of the main trunk slit. Line 69 is the center line of the main slit 6.

  Further, in order to take out one cell assembly from one edge 10 through the branch trunk slit 7 and the main slit 6 in a state where all the plurality of cell assemblies are attached to the substrate 5, one cell assembly It arrange | positions so that it may not contact with another cell assembly. Such a non-contact arrangement is achieved by arranging the tips of the branch trunk slits at a sufficient distance. It can also be achieved by providing a space between the branch trunk slit tips as described below or adopting the shape of the slit intersection.

Such a non-contact arrangement will be described with reference to FIGS.
FIG. 5 shows an example in which the distance between the tip ends (51, 54) of the branch stem slits located on both sides of the main slit 6 is larger than twice the diameter of the cell unit. In the cell assembly arranged at the distal end portion 51 of the branch trunk slit, the conducting tube 15a, the joint 29a, and the pressure sensor 17a are indicated by broken lines. Further, in the cell assembly arranged at the distal end portion 52 of the branch trunk slit, the joint 29b having a high possibility of contacting the pressure sensor 17a is indicated by a broken line. The cell assembly (that is, the conducting tube 15a) located at the tip 51 of the branch trunk slit 7a is moved from the branch trunk slit 7a through the intersection of the main slit 6 to the opposite branch trunk slit 7b in the normal arrangement state. Let When the cell assembly is rotated in the direction of the arrow 65, the cell assembly can be rotated without coming into contact with other cell assemblies. Then, the conducting tube 15 a is returned to the main slit 6. The cell assembly can be removed by passing through the main slit 6 with the pressure sensor 17a in the horizontal direction of the drawing.

  FIG. 6 is an example in which the corners of the branch points of the main trunk slit 6 and the branch trunk slit are cut. Similarly to FIG. 5, in the cell assembly disposed at the tip 51 of the branch trunk slit, the conducting tube 15a, the joint 29a, and the pressure sensor 17a are indicated by broken lines. Further, in the cell assembly arranged at the distal end portion 52 of the branch trunk slit, the joint 29b having a high possibility of contacting the pressure sensor 17a is indicated by a broken line. The cell assembly (that is, the conducting tube 15a) located at the distal end portion 51 of the branch trunk slit 7a is moved from the branch trunk slit 7 to the intersection of the main slit 6 in a normally arranged state. When the conduction tube 15a is positioned at the cut corner (lower left side of the drawing) and the cell assembly is rotated in the direction of the arrow 66, the cell assembly can be rotated without contact with other cell assemblies. Then, the cell assembly can be removed by passing through the main slit 6 in a state where the pressure sensor 17a is in the horizontal direction of the drawing.

  In this embodiment, the main trunk slit 6 and the branch trunk slit 7 intersect at an angle of 90 degrees, but can intersect at an arbitrary angle. Further, the main trunk slit 6 and the branch trunk slit 7 are not limited to straight lines, but can be arbitrary curves.

Referring to FIG. 3, four sub vacuum manifolds 26a, 26b, 26c, and 26d are attached to the upper surface of the bottom surface of base 4. Each sub-vacuum manifold is connected to a vacuum manifold 25 via an on-off valve 41, 42, 43, 44, and its tip 45 is connected to a vacuum pump (not shown). The four sub vacuum manifolds 26a, 26b, 26c, and 26d can be evacuated independently by opening and closing the on-off valves 41, 42, 43, and 44, respectively.
Each of the four sub-vacuum manifolds has five columnar vacuum connection ports 27a, 27b, 27c, 27d, and 27e, but the sub-vacuum manifolds 26b, 26c, and 26d are not shown.

  The measurement of the transmission amount using the multi-cell transmission amount measuring apparatus according to the present invention is usually performed as follows. Attach multiple cell assemblies to the base. Start the temperature control of the cell unit. The first on-off valve 16 and the second on-off valve 18 are closed, the vacuum pump is operated, and the vacuum manifold 25 and the sub vacuum manifold 26 are evacuated.

  The upper cell 11 is removed, the film to be tested is positioned in the lower cell 14, and the film to be tested is attached and fixed between the upper cell 11 and the lower cell 14. The first on-off valve 16 and the second on-off valve 18 are opened, and the inside of the lower cell 14 and the pressure sensor 17 is evacuated. A test gas or a test solution is supplied from the gas supply manifold 21 to the upper cell 11.

  When the measured value of the pressure gauge becomes constant, the second on-off valve 18 is closed. Since the gas that has permeated the film to be tested moves to the lower cell 14 and the measured value of the pressure sensor 17 increases, a permeation curve is obtained using that value as a function of time. The measurement is continued as it is until the permeation curve becomes a straight line, and the permeability, permeation count, moisture permeation, and the like are obtained from the calculation formula using the slope of the straight line portion of the permeation curve. Such a calculation is performed by the control device using software input in advance.

  The multi-cell permeation amount measuring device according to the present invention can be used as a device for measuring the permeation amount of gas or liquid that permeates a film or the like.

It is a partial cross section explanatory drawing of a multiple cell permeation amount measuring apparatus. It is surface explanatory drawing of a multiple cell permeation | transmission amount measuring apparatus. It is a perspective explanatory view of the base of the multiple cell permeation amount measuring apparatus. FIG. 3 is a perspective explanatory view of the cell assembly 3. It is an enlarged surface explanatory view of the main trunk slit 6 and the branch trunk slit 7. It is an enlarged surface explanatory drawing explaining the shape of the branch point of the main trunk slit 6 and the branch trunk slit 7. FIG.

Explanation of symbols

3 Cell assembly 4 Base 5 Substrate 6 Main stem slit 7 Handle stem slit 9 Cell unit 11 Upper cell 14 Lower cell 15 Conducting pipe 16 First on-off valve 17 Pressure sensor 18 Second on-off valve 20 Temperature controller 21 Gas supply manu Hold 23 Gas exhaust manifold 25 Vacuum manifold 26 Sub vacuum manifold 28 Vacuum joint

Claims (5)

It is composed of a plurality of cell assemblies, a vacuum manifold having a plurality of vacuum connection ports, and a control device.
The cell assembly includes a cell unit composed of an upper cell and a lower cell sandwiching a film to be measured for measuring the amount of permeation, a conducting tube extending downward from the lower surface of the lower cell, and sequentially downward to the other end of the conducting tube. Comprising a first on-off valve, a pressure sensor, a second on-off valve and a vacuum joint,
The vacuum joint is detachably connected to the vacuum connection port,
The multi-cell permeation amount measuring device, wherein the control device controls opening and closing of the first on-off valve and the second on-off valve. A gas supply manifold having a plurality of gas supply connection ports; a gas discharge manifold having a plurality of gas discharge connection ports;
The upper cell has a gas inlet joint and a gas outlet joint;
The gas introduction joint is detachably connected to the gas supply connection port,
The multi-cell permeation amount measuring apparatus according to claim 1, wherein the gas outlet joint is detachably connected to the gas discharge connection port. A base for disposing the plurality of cell assemblies, the vacuum manifold being disposed, and a substrate disposed in a horizontal direction in an upper space of the vacuum manifold;
The substrate is opened at one edge of the substrate, provided with a main slit through which the conducting pipe can pass, branched from the main slit, and provided with a plurality of branch stem slits through which the conducting pipe can pass,
The conducting tube is sent from the opening to the main trunk slit through the branch pipe slit of the cell assembly through the branch trunk slit to the tip of the branch trunk slit, and the cell assembly is disposed at that position. ,
The cell unit has a cylindrical shape,
The leading ends of the branch trunk slits are spaced apart from each other by a distance equal to or larger than the diameter of the cell unit, and the leading ends of the branch trunk slits are spaced from the center line of the main trunk slit by a distance equal to or larger than the diameter of the cell unit. A plurality of cell assemblies are arranged on a base having a substrate that is arranged separately,
Further, from the state in which the plurality of cell assemblies are arranged, the individual cell assemblies in the plurality of cell assemblies pass through the branch stem slit and the main slit without contacting the remaining plurality of cell assemblies. The multi-cell permeation amount measuring apparatus according to claim 1, wherein the plurality of cell assemblies are arranged in a state where they can be taken out from one edge of the substrate. 4. The vacuum manifold has n vacuum connection ports (n is a positive integer not less than 2 and not more than 10), and is branched to a sub-vacuum manifold having an opening / closing valve at a branch point. The multi-cell permeation amount measuring apparatus according to any one of the above. The multi-cell permeation amount measuring device according to any one of claims 1 to 4, wherein the cell unit has a temperature control means.

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