JP2010260557A - Method for manufacturing gas adsorbing device, and gas adsorbing device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To manufacture a gas adsorbing device capable of suppressing the determine of a gas adsorbing material, and preventing any through-hole from being formed in a container. <P>SOLUTION: After a gas adsorbing material 14 is filled in a gas hardly-permeable container 7 from an opening 8 of the gas hardly-permeable container 7 composed of a cylindrical metal member with one end opened, and the other end sealed, a lid material 11 having a substantially projecting longitudinal section composed of a bar-like part 12 with its outside diameter smaller than the inside diameter of the opening 8 and a flange 13 with its outside diameter larger than the inside diameter of the opening 8 is mounted to the gas hardly-permeable container 7 so that the bar-like part 12 is accommodated in the opening 8. An annular brazing filler metal 5 is installed close to a gap between an open end of the gas hardly-permeable container 7 and the flange 13 with the flange 13 side downwardly in the direction of gravity. The brazing filler metal 5 and its peripheral part are heated. After the brazing filler metal 5 is melted, and the brazing filler metal flows into a space between the gas hardly-permeable container 7 and the bar-like part 12 of the lid material 11 due to a capillary phenomenon, the brazing filler metal is cooled and solidified to seal the opening 8 of the gas hardly-permeable container 7. <P>COPYRIGHT: (C)2011,JPO&amp;INPIT

Description

  The present invention relates to a gas adsorption device in which a container is filled with a gas adsorbent, and more particularly to sealing of an opening of a container after the gas adsorbent is filled in the container.

  In recent years, development of devices (hereinafter referred to as vacuum devices) capable of exhibiting performance in an advanced vacuum environment, such as vacuum heat insulating materials, vacuum heat insulating containers, and plasma display panels, has become active.

  For these vacuum devices, an increase in internal pressure due to residual gas at the time of manufacture or gas that enters over time causes deterioration in performance. Therefore, application of gas adsorbents for adsorbing these gases has been attempted.

  When the gas adsorbent comes into contact with air in the atmosphere, the gas adsorbent adsorbs air, resulting in a reduction in gas adsorption capacity. Thus, attempts have been made to cover with a gas poorly permeable container or a gas permeable material (see, for example, Patent Document 1).

  In addition, when heat treatment is required to exert the adsorption performance of the gas adsorbent, in order to seal the gas adsorbent with a gas impermeable container, set the gas impermeable container and the brazing material in advance as a set. A method of melting and brazing the brazing material in the same process as the heat treatment of the gas adsorbent by installing in a heat treatment furnace and raising the temperature is effective.

  As a conventional brazing method, there is one disclosed in Patent Document 2, for example. Hereinafter, a conventional brazing method will be described with reference to FIG.

  As shown in FIG. 4 (a), the inner container 1 and the outer container 3 provided with the exhaust hole 2 are joined at the end part 4 to form a double structure, with the exhaust port 2 facing upward, 5 is disposed, and the sealing plate 6 is placed on the brazing material 5 and then vacuum heat treatment is performed in a vacuum heating furnace, and the space formed by the inner container 1 and the outer container 3 is evacuated and then brazed. By softening the material 5, the sealing plate 6 is brought close to the outer container 3 by its own weight, and the exhaust hole 2 is sealed by making the state shown in FIG. 4B.

Japanese National Patent Publication No. 9-512088 JP 58-192516 A

  However, in the method described in Patent Document 1, the gas barrier property of the gas-impermeable material covering the gas adsorbent is not necessarily sufficient, and in the step of installing the gas adsorbent in the space where the gas to be adsorbed exists, Since the gas adsorbent adsorbs the surrounding gas, it was difficult to suppress the deterioration of the adsorbent.

  In general, brazing in the atmosphere is completed by quickly cooling the molten brazing material after the molten brazing material is attached to the member to be joined. On the other hand, in the method described in Patent Document 2, the outer container to be joined and the brazing material in a molten state are in contact with each other for a longer time than brazing in the air. It is said that the brazing material is in a molten state from the time when the temperature in the furnace reaches the melting point of the brazing material during heating until it falls below the melting point of the brazing material during cooling. This is because it takes much longer than the furnace.

  On the other hand, when different metals in the molten state or alloys with different compositions are held in contact with each other, a phenomenon occurs in which the constituent elements of each other mix and try to make uniform. When this phenomenon occurs during brazing between a cylindrical thin metal member having a different composition and a brazing material, the metal member is thin and thus a through hole may be generated. Therefore, originally, when brazing is performed in a vacuum heating furnace, it is not preferable that the members to be joined are thin.

  However, since the gas adsorption device needs to be opened inside the vacuum apparatus, the gas-impermeable container needs to be thin so that it can be easily opened.

  Therefore, the present invention suppresses the deterioration of the gas adsorbent in the gas adsorption device manufacturing process and the installation process in the space where the gas to be adsorbed exists, and does not cause a through-hole in the thin container. It aims at providing the preparation method of the gas adsorption device which has the outstanding gas barrier property.

  In order to achieve the above object, the gas adsorption device manufacturing method of the present invention is a hollow cylinder in which one end is open and the other end is sealed, and the length of the body part from one end to the other end is equal to or greater than the maximum width of the end part. After filling the gas adsorbent from the opening of the gas-impermeable container made of a thin metal member, the rod-shaped portion whose outer diameter is smaller than the inner diameter of the opening and the flange portion whose outer diameter is larger than the inner diameter of the opening A lid member having a substantially convex longitudinal section is attached to the gas-impermeable container so that the rod-shaped portion is accommodated in the opening, and the flange-side is directed downward in the direction of gravity so that the gas-impermeable container A brazing material is installed in the vicinity of the gap between the open end of the flange and the flange portion, the brazing material and its peripheral part are heated, and the brazing material is melted to cause the gas-impermeable permeable container and After flowing between the rod-shaped parts of the lid, cooling solid By is to seal the opening of the gas-impermeable container.

  According to this, the production of the gas adsorption device (sealing of the opening of the container) can be performed in vacuum, the deterioration of the gas adsorbent in the gas adsorption device production process is suppressed, and the gas adsorption during storage in the atmosphere It is possible to obtain a gas adsorption device that suppresses deterioration of the material.

  Furthermore, as shown below, it is possible to suppress the formation of through holes in the gas permeable container.

  The brazing material flows in between the gas-impermeable container and the rod-shaped portion of the lid material by capillary action, so that the brazing material takes in the elements constituting the gas-impermeable container and the lid material. Because the total amount of brazing material that can be incorporated into the element is limited, if the elements that make up the lid contain many of the same elements as the main elements of the gas permeable container, A large amount of this element is taken from both the permeable container. As a result, the contribution degree of the element taken in by the brazing material from the gas-impermeable container becomes small, and the formation of the through hole of the gas-impermeable container can be suppressed. As a result, a gas adsorption device having excellent gas barrier properties can be obtained.

  According to the method for producing a gas adsorption device of the present invention, gas adsorption capable of suppressing the deterioration of the gas adsorbent in the gas adsorption device production step and the step of installing the gas adsorption device in the space where the gas to be adsorbed exists. A device can be provided.

  Furthermore, a poorly gas permeable container that is produced when the composition of the molten brazing material is homogenized with the composition of the hardly gas permeable container by pouring a molten brazing material between the hardly gas permeable container and the lid. The formation of through-holes can be suppressed.

Schematic sectional view of the gas adsorption device before the heat treatment in the production process of the gas adsorption device of Embodiment 1 of the present invention Schematic sectional view of the gas adsorption device after the heat treatment in the production process of the gas adsorption device of the embodiment Characteristic diagram showing schematic state of binary alloy (A) Side view before brazing of conventional gas-impermeable container (b) Side view after brazing of the conventional gas-impermeable container

  According to a first aspect of the present invention, there is provided the gas permeable container comprising a hollow cylindrical thin-walled metal member having one end opened and the other end sealed, and the length of the body from one end to the other is not less than the maximum width of the end. After filling the gas adsorbent from the opening, the longitudinal section consisting of a rod-shaped portion whose outer diameter is smaller than the inner diameter of the opening and a flange portion whose outer diameter is larger than the inner diameter of the opening is a substantially convex lid. The rod-shaped part is attached to the gas-impermeable container so that the rod-shaped part fits in the opening, the flange part side is directed downward in the direction of gravity, and the gap between the opened end of the gas-impermeable container and the flange part After the brazing material is installed in the vicinity, the brazing material and its peripheral part are heated, and after the brazing material is melted and flows between the gas-impermeable container and the rod-shaped part of the lid material by capillary action, By cooling and solidifying, the opening of the gas permeable container A method for manufacturing a gas adsorption device for sealing.

  If the gas adsorbent is exposed to a gas other than the intended purpose before use, the gas will be adsorbed and the adsorption capacity will be reduced (deteriorated) or the adsorption capacity will be lost (deactivated). It is necessary to enclose in a gas adsorption device that does not come into contact with outside air. Therefore, one of the important functions of the gas adsorption device is to suppress the contact with the gas until the time of use and maintain the gas adsorption ability of the gas adsorbent.

  Therefore, the production of the gas adsorbing material has to be performed in a vacuum or in an inert gas such as argon, which the gas adsorbing material cannot adsorb.

  In general, it is often carried out in a glove box filled with an inert gas such as argon, but the workability is poor, handling takes time, and the consumption of argon gas is large. It was an unfavorable condition. Another problem is that the gas adsorbent deteriorates due to the presence of impurity gas such as air that has entered from the outside in the glove box.

  In the method for producing a gas adsorbing device according to this configuration, as an example, the gas adsorbing device can be produced while suppressing deterioration of the gas adsorbent that deteriorates or deactivates when exposed to the atmosphere after being activated by vacuum heat treatment. it can.

  That is, according to the method for producing a gas adsorbing device according to the present configuration, the gas-impermeable container filled with the gas adsorbing material can be sealed only by heating without contacting the outside. Therefore, it becomes possible to seal a gas-impermeable container without performing an operation in a glove box filled with an inert gas, that is, to produce a gas adsorption device. The running cost increase due to the use of inert gas can be suppressed.

  In addition, by installing a brazing material in the vicinity of the opening in which the lid made of a rod-shaped portion is installed, the brazing material heated and melted flows between the gas-impermeable container and the lid, and the opening is sealed. While being able to stop, the sealing loss of the gas poorly permeable container by the through-hole production | generation by brazing material can be reduced.

  This effect will be described below.

  In general, since the composition of the hardly gas permeable container and the composition of the brazing material are different, when the brazing material is melted, a phenomenon occurs in which the composition of the hardly gas permeable container and the composition of the brazing material become uniform. This phenomenon occurs strongly when the composition of the gas permeable container and the composition of the brazing material are greatly different. For example, when the gas hardly permeable container is pure aluminum and the brazing material is an alloy of aluminum and silicon, the brazing material takes in the aluminum of the gas hardly permeable container and a through hole is formed in the gas hardly permeable container.

  However, in the present invention, no through hole is generated for the following reason.

  The brazing material flows by capillary action between the gas-impermeable container and the rod-shaped portion of the lid material, thereby taking in the substances constituting the gas-impermeable container and the lid material. However, since the total amount that the brazing material can take in the substance is limited, if the substance that constitutes the lid material contains many elements that are the same as the main element of the substance that constitutes the gas permeable container, the brazing material Takes in a lot of this element from both the lid and the gas-impermeable container. As a result, the contribution of the substance taken in by the brazing material from the gas permeable container becomes small, and the formation of through holes in the gas permeable container can be suppressed. As a result, a gas adsorption device having excellent gas barrier properties can be obtained.

  As a result, a gas adsorption device having excellent gas barrier properties can be obtained.

  Furthermore, by installing a brazing material at the peripheral boundary between the flange and the opening, the cost of manufacturing the gas adsorption device can be reduced, and this factor is as follows.

  In order to install the brazing material at the peripheral boundary between the flange and the opening, it is necessary to fix the brazing material at the above position. For example, if the shape of the brazing material is an annular shape whose inner diameter is larger than the outer diameter of the end portion having the opening of the gas permeable container and smaller than the outer diameter of the flange portion, the hollow portion of the annular brazing material When the gas poorly permeable container is passed through and the flange portion is installed as the bottom portion, the flange portion is automatically contacted and fixed by gravity. In this way, the brazing material is installed at the peripheral boundary between the flange and the opening.

  Therefore, the installation of the brazing material does not require a complicated operation, and the operation can be completed promptly.

  Here, the end portion is a boundary portion with the periphery in the longest direction of the cylindrical member, and the bottom surface and the top surface correspond to this.

  The opening is a portion where the inside and outside of the hollow gas permeable container can be connected without passing through the constituent material of the gas permeable container, and from here the gas adsorbent can be filled. .

  The trunk portion is a portion constituting most of the cylindrical member, and is a portion from a portion of about 5 mm from one end portion to a portion of about 5 mm from the other end portion.

  A cylindrical shape is an object that is long in one direction and is hollow.

Here, the poorly gas permeable container means that the gas permeability of the container is 10 ⁴ [cm ³ / m ² · day · atm] or less, more desirably 10 ³ [cm ³ / m ² · day.atm].

  Moreover, although the metal which comprises a gas poorly permeable container is not specified in particular, iron, copper, aluminum etc. can be used, for example. An alloy such as an aluminum alloy or a copper alloy can also be used.

  The gas adsorbent can adsorb non-condensable gas contained in the gas. Although not specified in particular, CuZSM-5 obtained by ion exchange of ZSM-5 zeolite with copper, oxides of alkali metals and alkaline earth metals, hydroxides of alkali metals and alkaline earth metals, etc. are used. In particular, there are lithium oxide, lithium hydroxide, barium oxide, barium hydroxide and the like.

  Further, after the gas adsorption device is installed in the space where the gas to be adsorbed exists, it is necessary to destroy the gas-impermeable container and ensure the air permeability so that the external gas can be adsorbed. Therefore, the thickness of the gas adsorbing device container material is desirably thin enough to be easily broken by pressing a projection such as a thumbtack at atmospheric pressure when installed in a vacuum heat insulating material. For example, in the case of aluminum, it may be 1 mm or less, desirably 0.5 mm or less, and more desirably 0.15 mm or less.

  The brazing material may be any material that can seal the hardly gas permeable container by being melted by heat and then cooled and solidified. And what is necessary is just to be able to make the gas passage amount of a sealing part small to the same extent as the gas passage amount of a gas poorly permeable container.

  The brazing material is generally an alloy material and is not particularly specified, but copper brazing, aluminum brazing, or the like can be used.

  The melting temperature of the brazing material is preferably lower by 30 ° C. or more than the melting temperature of aluminum from the viewpoint of temperature control, but this is not the case when precise temperature control is possible.

  The temperature control conditions for cooling and solidification are not particularly specified, and natural cooling in the heating furnace can be performed. In addition, when the gas permeable container is thick and difficult to break, it can be cooled at about 300 ° C./h in order to perform softening by annealing. Furthermore, when the gas permeable container is thin and can be easily broken, it may be cooled at about 10 ° C./min in order to improve the productivity of the gas adsorption device.

  With the above configuration, the gas adsorbent that adsorbs, deteriorates, or deactivates when exposed to unintended gas is sealed so that it does not come into contact with unintended gas. Thus, it is possible to provide a gas adsorption device that can reduce deterioration during storage from production to use and when applied to vacuum equipment at low cost.

  Further, by providing a gas adsorbing device in which deterioration of the gas adsorbing material is reduced even when stored for a long period of time by suppressing the formation of through holes in the gas permeable container by the brazing material and ensuring excellent gas barrier properties. be able to.

  In a second aspect of the invention, in particular, in the first aspect of the invention, the gas-impermeable container is made of aluminum or an alloy mainly composed of aluminum, and the brazing material is made of an alloy made of aluminum and silicon.

  Since aluminum is soft and easy to break after being installed in a vacuum device, it is possible to obtain a gas adsorbing device with excellent handleability.

  Further, an alloy brazing material made of aluminum and silicon is suitable because it has excellent affinity with aluminum or aluminum alloy used as a gas-impermeable container.

  With the above configuration, it is possible to obtain a gas adsorption device capable of suppressing the deterioration of the gas adsorbent in the gas adsorption device manufacturing process and the process of installing the gas adsorption device in the space where the gas to be adsorbed exists. By simultaneously performing heating of the adsorbent and heating of the brazing material, it is possible to reduce facility operating power and man-hours required for manufacturing the gas adsorbing device, and to reduce the cost of manufacturing the gas adsorbing device.

  In the third invention, in particular, in the first or second invention, the maximum distance from the flange portion of the brazing material after solidification is larger than the maximum distance from the flange portion of the brazing material before melting.

  Since the maximum distance from the flange portion of the brazing material after solidification is higher than the maximum distance from the flange portion of the brazing material before melting, through holes are generated near the opening of the gas-impermeable container due to erosion of the brazing material. However, it is possible to form a sealed space and obtain a gas permeable container having excellent gas barrier properties.

  A fourth invention is a gas adsorption device produced by the method for producing a gas adsorption device according to any one of the first to third inventions.

  In the manufacturing process, since the gas adsorbent is hardly deteriorated, it has excellent gas adsorption characteristics. Furthermore, in the case of using a gas adsorbing material that requires heat treatment for activation, heat treatment and sealing in a gas hardly permeable container can be performed in the same process, and thus there is a feature that it is inexpensive.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. Note that the present invention is not limited to the embodiments.

(Embodiment 1)
FIG. 1 is a schematic cross-sectional view of a gas adsorption device before heat treatment in the gas adsorption device fabrication process of Embodiment 1 of the present invention, and FIG. 2 is a gas after heat treatment in the gas adsorption device fabrication process of the same embodiment. It is a schematic sectional drawing of an adsorption device.

  1 and 2, the gas permeable container 7 is made of metal and has a circular opening 8 at one end. The distance between the ends of the gas permeable container 7 (the length of the body 9) is 120 mm, the wall thickness of the body 9 is 0.10 mm, and the sealing surface 10 at the end opposite to the opening 8 is used. Has a cylindrical shape with a thickness of 1 mm and an inner diameter of 10 mm.

  Moreover, the rod-shaped part 12 of the cover material 11 is inserted into the opening part 8, and the flange part 13 of the cover material 11 and the edge part by the side of the opening part 8 contact.

  Here, the rod-shaped portion 12 of the lid member 11 has a cylindrical shape with a diameter of 9.9 mm and a height of 5 mm. Further, the flange portion 13 of the lid member 11 has a cylindrical shape having a diameter of 15 mm and a height of 1 mm.

  In addition, a filter 15 made of an aggregate of heat-resistant fibers is installed between the lid member 11 and the air adsorbent 13 in order to prevent the gas adsorbent 14 from scattering. Further, a brazing material 5 obtained by processing a rod-like member having a diameter of 1.5 mm and a length of 35 mm into a circular shape is installed on the upper portion of the flange portion 13.

  A method for manufacturing the gas adsorption device of the present embodiment configured as described above will be described below.

  1 g of gas adsorbent 14 which shows activity by heat treatment, for example, powdery CuZSM-5 which is ZSM-5 zeolite ion-exchanged with copper, is filled in the gas impermeable container 7 shown in FIG. A filter 15 made of wool is installed in the gas permeable container 7. Here, rock wool is used for the filter 15, but it is only required to have heat resistance and low gas generation, and inorganic fibers such as alumina fibers and quartz fibers, and metal fibers such as steel wool can be used.

  This series of operations is carried out with the sealing surface 10 at the sealed end facing downward in the direction of gravity so that the gas adsorbent 14 filled in the gas impermeable container 7 does not spill, but the filter 15 is installed. After that, the gas adsorbent 14 is not spilled by the filter 15, so that the direction can be freely determined.

  After the filter 15 is installed, the rod-like portion 12 of the lid member 11 is inserted into the opening 8 and brought into contact with the flange portion 13. Next, in this state, the lid member 11 is placed downward and the sealing surface 10 is placed upward, and the brazing material 5 is brought into contact with the flange portion 13 through the brazing material 5 from the lower portion 10 side.

  In this state, the gas hardly permeable container 7, the gas adsorbing material 14, and the brazing material 5 are installed in a vacuum heating furnace (not shown). After depressurizing the vacuum heating furnace to 0.01 Pa, the temperature was raised to the solidus temperature of the brazing material. At this time, the gas inside the gas permeable container 7 is discharged from between the opening 8 and the rod-shaped portion 12.

  In the binary alloy, at a temperature below the solidus temperature, a state in which the first component metal is present alone in the solid solution composed of the first component element and the second component element can be taken. The mechanism by which the alloy in such a state melts is as follows.

  First, a characteristic diagram showing the state of the binary alloy is shown in FIG.

  The case where the brazing material 5 is a hypoeutectic alloy in which the ratio of the first component is larger than the eutectic point in FIG. 3 will be described. However, the present invention is not limited to the hypoeutectic alloy, and eutectic alloy and hypereutectic alloy are used. You can also.

  In this description, a solid component is described as a first component S and a second component S, and a liquid component is described as a first component L and a second component L.

  A hypoeutectic alloy takes a state in which a solid solution composed of a first component S and a second component S and a single first component S are mixed below the solidus temperature, and the temperature of the alloy rises to increase the solid phase. When the line temperature is reached, the solid solution portion melts and the first component S is deposited in the liquid composed of the first component L and the second component L.

  When the temperature further rises, the metal of the first component S dissolves in the first component L and the second component L that have been melted into a liquid. As a result, the ratio of the metal of the first component L contained in the portion that has melted to become a liquid increases.

  When the temperature further rises, the metal of the first component S dissolves into the completely liquid portion, the first component S disappears, and the entire alloy becomes a uniform liquid. This temperature is the liquidus temperature.

  According to the ratio of the first component and the second component in the composition of the entire alloy, the temperature at which the element of the first component is completely taken into the liquid part, that is, the liquidus temperature differs, and this temperature is different for each composition of the entire alloy. What is connected is a liquidus line in the state diagram.

  Therefore, in the state heated above the solidus temperature and below the liquidus temperature, the brazing material 5 is in a semi-molten state in which the ratio is large in the alloy liquid, that is, the first component is precipitated. A part of the semi-molten brazing material 5 having a low melting point melts and flows between the opening 8 and the rod-like part 12 by capillary action. Further, by cooling the vacuum heating furnace, the brazing material 5 is solidified and sealed.

  After the brazing material 5 is solidified, the vicinity of the opening 8 has been eroded and thinned by the brazing material 5, but the brazing material 5 flows into the extent that it completely covers the rod-like portion 12, and the body of the gas permeable container 7. The part 8 and the lid member 11 were joined, and the gas adsorbent could be sealed.

  By slowing down the cooling rate at this time, the metal constituting the gas permeable container 7 is annealed and becomes flexible. Therefore, the destruction when installed in the space where the gas to be adsorbed is facilitated. Further, when the gas adsorption device was taken out from the vacuum heat treatment furnace and opened to the atmosphere, the gas adsorption device was compressed by atmospheric pressure. Therefore, the thickness of the thinnest portion filled with the gas adsorption material was 5 mm.

  The manufacturing method of the gas adsorption device according to the present embodiment is such that a hollow cylindrical thin metal member having one end opened and the other end sealed, and the length of the body portion 9 from one end to the other end is equal to or greater than the maximum width of the end portion. The gas adsorbent 14 is filled into the gas impermeable container 7 through the opening 8 of the gas impermeable container 7, and the filter 15 is inserted into the gas impermeable container 7. After preventing from coming out of the opening 8 of the gas permeable container 7, a longitudinal section composed of the rod-shaped portion 12 whose outer diameter is smaller than the inner diameter of the opening 8 and the flange portion 13 whose outer diameter is larger than the inner diameter of the opening 8 is formed. The substantially convex lid member 11 is attached to the gas-impermeable container 7 so that the rod-shaped portion 12 is accommodated in the opening 8, and the opening of the gas-impermeable container 7 is made with the flange portion 13 facing downward in the gravity direction. Close to the gap between the end (opening 8 side end) and the flange 13 An annular brazing material 5 is installed, the brazing material 5 and its peripheral part are heated, and the brazing material 5 is melted and flows between the gas-impermeable container 7 and the rod-shaped part 12 of the lid material 11 by capillary action. Thereafter, the opening 8 of the gas permeable container 7 is sealed by cooling and solidifying.

  When the air adsorption amount of the gas adsorption device produced as described above was measured 1 hour after production, the adsorption amount was 5 cc / g at an adsorption equilibrium pressure of 10 Pa. Moreover, when the same measurement was performed 30 days after production, the amount of adsorption was 5 cc / g at an adsorption equilibrium pressure of 10 Pa. As a result, it can be seen that the gas adsorption device produced by the gas adsorption device production method of the present embodiment does not deteriorate in performance even when stored for a long period of time.

  When the gas permeable container 7 is disassembled after the adsorption amount is measured and the vicinity of the lid material 11 is examined, the brazing material 5 completely covers the lid material 11 and the maximum distance from the flange portion 13 to the brazing material 5 is 5 mm. It was. At the beginning of installing the brazing material 5 on the flange portion 13, the maximum distance of the brazing material 5 from the flange portion 13 is 1.5 mm because it is the diameter of the cross section of the brazing material 5. From this, it was found that the brazing material 5 was sealed by covering the upper surface of the rod-shaped portion 12 by flowing between the gas-permeable container 7 and the rod-shaped portion 12.

Example 1
In the configuration of the first embodiment, the case where the gas-impermeable container 7 and the lid material 11 are pure aluminum and the brazing material 5 is an alloy of aluminum and silicon will be described.

  When the temperature in the vacuum heating furnace rises and reaches the solidus temperature, the brazing material 5 placed on the upper portion of the flange portion 13 starts to melt. At the start of melting, the portion containing a relatively large amount of silicon is melted, the portion containing a relatively small amount of silicon is not melted, and the solid phase and the liquid phase are mixed. In this state, since the melted portion contains a large amount of silicon, when it comes into contact with aluminum, the aluminum is eroded. For this reason, when installed in a vacuum device, the vicinity of the opening 8 of the gas permeable container 7, which is thin so that it can be easily broken, may be eroded and a through hole may be formed.

  Further, the melted brazing material 5 flows between the rod-like portion 12 of the lid member 11 and the gas hardly permeable container 7 by capillary action. The brazing material 5 that has flowed between the rod-shaped portion 12 of the lid member 11 and the hardly gas permeable container 7 erodes the aluminum constituting the rod-like portion 12 of the lid member 11 and the aluminum constituting the hardly gas permeable container 7. However, it reaches a part away from the opening 12.

  The brazing material 5 gradually erodes the aluminum by eroding the aluminum of the gas permeable container 7 and the lid 11. As a result, even if the gas poorly permeable container 7 is contacted, a through hole of the gas hardly permeable container 7 due to the erosion of the brazing material 5 is not generated in a portion away from the opening 8.

  Through the above process, a sealed space is formed by the gas permeable container 7, the lid member 11, and the brazing material 5, and a gas adsorption device can be obtained.

  When the air adsorption amount of the gas adsorption device produced as described above was measured 1 hour after production, the adsorption amount was 5 cc / g at an adsorption equilibrium pressure of 10 Pa. Moreover, when the same measurement was performed 30 days after production, the adsorption amount was 5 cc / g at an adsorption equilibrium pressure of 10 Pa. As a result, it is understood that the performance of the gas adsorption device does not deteriorate even when stored for a long time.

  Although the case of pure aluminum as the gas permeable container 7 and the lid 11 and the alloy of aluminum and silicon as the brazing material 5 is shown, it is not limited to these, and metals such as copper and iron can be used. is there.

  Here, pure aluminum includes 99% or more of aluminum.

  A gas adsorption device manufacturing method and a gas adsorption device according to the present invention include a gas adsorption device that suppresses deterioration of a gas adsorbent that loses adsorption characteristics when exposed to air in a production process. This can be achieved without installation, and a gas adsorption device can be obtained at low cost. Furthermore, heat treatment is required to develop gas adsorption ability, and after heat treatment, it can be used for heat treatment and sealing of chemicals that deteriorate when touched by gas.

DESCRIPTION OF SYMBOLS 5 Brazing material 7 Gas | liquid hardly permeable container 8 Opening part 9 Body part 10 Sealing surface 11 Cover material 12 Rod-shaped part 13 Flange part 14 Gas adsorbent

Claims (4)

A gas adsorbent from the opening of the gas-impermeable container made of a hollow cylindrical thin-walled metal member having one end opened and the other end sealed and the length of the body from one end to the other being equal to or greater than the maximum width of the end A lid having a substantially convex cross-section comprising a rod-shaped portion whose outer diameter is smaller than the inner diameter of the opening and a flange portion whose outer diameter is larger than the inner diameter of the opening, and the rod-shaped portion is located inside the opening. The brazing material is attached to the hardly gas permeable container so that it fits in, the flange part side is directed downward in the direction of gravity, and close to the gap between the open end of the hardly gas permeable container and the flange part. By installing, heating the brazing material and its peripheral portion, the brazing material melts and flows between the gas-impermeable container and the rod-shaped portion of the lid material by capillary phenomenon, and then solidifies by cooling. Gas that seals the opening of the gas permeable container A manufacturing method of wearing the device. The method for producing a gas adsorption device according to claim 1, wherein the gas-impermeable container is aluminum or an alloy containing aluminum as a main component, and the brazing material is an alloy composed of aluminum and silicon. The method for producing a gas adsorption device according to claim 1 or 2, wherein the maximum distance from the flange portion of the brazing material after solidification is greater than the maximum distance from the flange portion of the brazing material before melting. A gas adsorption device produced by the method for producing a gas adsorption device according to any one of claims 1 to 3.

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