Process chamber for filling and sealing a hollow glass body, method therefor and glass capsule

Abstract

The invention relates to a process chamber (10) having a filling space (11), a process space (12) and a cooling space (40) for filling and sealing a hollow glass body (20) with a radioactive filling gas (23). The filling space (11) can be connected to a vacuum pump (31a) and to a pressure control device (32a), for filling the filling space (11) with the filling gas (23) up to a filling pressure (P1), and for removing residual filling gas (23), and to a pressure compensation valve (33a). The process space (12) has a pressure control device (32b) for achieving a predefined process pressure (P2) which is higher than the filling pressure (P1), and a pressure compensation valve (33b). A sealable feed-through (13a) for feeding through an open end region (21) of a hollow glass body (20) is formed between the filling space (11) and the process space (12). The process space (12) has a melting zone (16) with a heating means (17) for locally heating the hollow glass body (20) and has a passage (13b) from which a closed body (22) of the hollow glass body (20) can protrude, which is cooled in the cooling space (40). The invention also relates to a method for filling and sealing a hollow glass body (20) and to a filled and sealed glass capsule (25).

Description

[0001] Process chamber for filling and sealing a hollow glass body, method for doing so, and glass capsule

[0002] Description

[0003] The invention relates to a process chamber for filling and sealing a

[0004] The invention relates to five glass hollow bodies with an open end and a closed body, which, in use, are to be filled with a filling gas consisting of at least 50 vol% tritium, deuterium and / or protium at standard conditions (1 bar, 20°C) and sealed gas-tight. The invention also relates to a method for filling and sealing the body and to a glass capsule resulting therefrom.

[0005] 10 Technical Area

[0006] As an example of such a glass capsule, we will mention the GTLS, "Tritium Gaseous Light Sources." These tritium gas light sources have been manufactured since the 1950s. They consist of a hollow glass body filled with tritium gas. The inside of the glass body can be coated with a phosphorescent pigment beforehand.

[0007] Fifteen are needed to achieve the desired color. These glass capsules glow independently for over 20 years. They can be manufactured very small and are known, for example, as luminous dots in watches or as emergency exit markers; formerly, they were also used as instrument aids in aircraft cockpits so that pilots could operate the instruments even at night in the event of a sudden power outage.

[0008] 20. Because tritium gas is radioactive, its handling is strictly regulated. Furthermore, the seal must be absolutely airtight. Equally strict regulations apply to the handling and gas-tight sealing of the other gases used, deuterium and protium, and their mixtures, particularly due to the risk of explosion. The gases each serve as energy carriers, especially deuterium and protium. Tritium provides the energy to make the self-illuminating light sources glow, although this energy is less than that provided by deuterium and protium.

[0009] Other applications of such filled glass capsules include diamond batteries and fusion sources. In diamond batteries, single-crystal nanodiamonds are placed in a, for example, lens-shaped hollow glass disk and filled with gas to create a fusion reaction.

[0010] 30 subsequently to supply small amounts of electricity for between 9,000 and 28,000 years when loaded with C-14, or for approximately 100 years when loaded with tritium.

[0011] SSY-POl-WO GTLS glass capsules are one of the most important areas of application. Tritium gas is the energy carrier that releases the energy. The more gas is introduced into the glass body, the brighter it glows.

[0012] According to the state of the art, the hollow glass bodies, which usually have the shape of a

[0013] The glass container must be a 5-inch long tube, closed at one end, or at least designed as a tube in the area of ​​the filling opening, and sealed with a flame or electrically. The internal pressure during sealing must not exceed the ambient pressure to prevent the seam from bursting and the tritium gas from igniting in the air. Therefore, filling is usually carried out at an internal pressure of 350 to 950 mbar, lower than the ambient pressure. Additionally, part of the glass container can be cooled during the filling process. This allows the effective final pressure to be increased to a certain extent once room temperature is restored, according to Amontons' law. According to this law, the pressure p increases proportionally to the temperature increase T in Kelvin when the amount of substance n and the volume V are constant.

[0014] 15 US Patent 4,768,984 describes the manufacture of halogen lamps. For this purpose, a glass tube closed at one end, containing pre-made filaments held together in a glass bead, is placed in a suitable apparatus with essentially two chambers. The open end of the glass tube leads into a heated filling chamber into which pressurized gas is introduced. The remainder of the glass tube is located in a

[0015] The process chamber is sealed off from the filling chamber and is also pressurized. A controlled heating plate heats and seals the glass tube in the area of ​​the glass bead, so that the pressurized gas is trapped in the cavity of the glass tube containing the heating wire. This cavity is cooled to increase the gas density. A heat exchanger with a circulating coolant is located in the process chamber for cooling purposes.

[0016] A disadvantage of this device is its complicated design for inserting the blanks and removing the finished parts. Furthermore, the purely temperature-controlled process is prone to defects such as the sealing seam bursting if the filling pressure becomes too high due to the additional heating in the filling chamber, especially since the process chamber is...

[0017] 30. The cooling system is additionally cooled, which lowers the pressure within it. Finally, the direct proximity between the cooling system and the controlled heating plate is disadvantageous for process control.

[0018] In Ellefson's publication RE: "High-pressure bulk-phosphor tritium lamps", 1990, a phosphorus-coated tritium lamp with an internal pressure of 7.1 bar is disclosed.

[0019] SSY-POl-WO Documents US 4213052 A and US 4273398 A each describe a flat glass tube that is heated by a laser until it plasticizes and is then sealed. The glass capsules contain radioactive gases under pressure.

[0020] Description of the invention

[0021] 5. The object of the present invention is to describe a process chamber as set forth above, with which the filling quantity of the aforementioned filling gases, or more generally with radioactive and / or explosive gases, in a gas capsule can be further increased, or which, with the same filling quantity, can be manufactured more simply and thus more cost-effectively. Furthermore, a method for filling and sealing such a hollow glass body is to be described, as well as a glass capsule filled and sealed by this method. Since the glass capsules are to be filled with radioactive tritium and / or explosive deuterium and / or protium, a high level of process reliability is required. For safety reasons, the bursting of a glass tube during sealing must be reliably prevented.

[0022] 15 The problems are solved by the features in the independent claims in the respective categories. According to the invention, the process chamber has a filling chamber and a process chamber, which are each gas-tight and pressure-resistant during use, also from each other. Thus, each of these chambers can be pressurized to a different predetermined pressure.

[0023] 20. The filling chamber can be connected to a vacuum pump for emptying the chamber and to a pressure regulating device. This pressure regulating device, in turn, can be connected to a filling gas container for filling the chamber with the filling gas up to a predetermined filling pressure > 1,000 mbar or even higher than the ambient pressure, which is assumed to be approximately 1,000 mbar. The pressure regulating device also allows for the extraction of residual filling gas from the filling chamber, preferably for its return to the filling gas container. Furthermore, the filling chamber has a pressure equalization valve to achieve ambient pressure in the emptied filling chamber. The vacuum pump and the pressure equalization valve can be designed as a single component.

[0024] The process chamber can be connected to a pressure regulating device to achieve a

[0025] The process chamber is designed with a predetermined process pressure that is higher than the filling pressure, and a pressure equalization valve is used to equalize the process chamber to ambient pressure. Therefore, the process chamber must also be designed in such a way as to withstand any process-induced overpressure in the process chamber relative to the filling chamber, especially if they share a common partition.

[0026] SSY-POl-WO The process chamber should be equipped with at least the aforementioned connections to allow for the tight, pressure-tested, and safe connection of the components for the pressure devices, which may also be combined. For the process to be carried out, the aforementioned components must be attached to the process chamber.

[0027] 5. A pressure-tight sealable passage is provided between the filling chamber and the process chamber, allowing an open end section of the glass body to pass from the process chamber into the filling chamber. During use, the opening of the glass body should be positioned with part of the end section of the glass cavity in the filling chamber, while the remainder of the end section and at least part of the remaining glass cavity are located in the process chamber.

[0028] Furthermore, the process chamber features a melting zone with a heating medium for locally heating the hollow glass body within this zone until it reaches its local plastic deformability. The melting zone is defined as the area where the heating medium can generate localized heating during use.

[0029] 15 According to the invention, the process chamber has a pressure-tight sealable passage from which the closed body of the gas hollow body protrudes during use. Furthermore, the process chamber has an additional cooling chamber outside the process chamber for enclosing and cooling a closed body of the glass hollow body protruding from the process chamber, the cooling chamber preferably being equipped with

[0030] The cooling chamber is cooled with liquid nitrogen. For example, it is a well-insulated container with a mirrored interior, similar to Dewar flasks. The coolant, such as liquid nitrogen, is therefore in direct contact with the glass container to achieve optimal cooling. This makes the cooling process more efficient than using a heat exchanger.

[0031] 25 The passage can be sealed to the glass body in the same way as the feedthrough.

[0032] The following describes the inventive method for filling a hollow glass body with a filling gas consisting of at least 50 vol% tritium, deuterium and / or protium under standard conditions (1 bar, 20°C), as well as the gas-tight sealing of the

[0033] 30 glass bodies are used to form a glass capsule. This involves using a process chamber as described above and a glass body with a closed body and an open end for filling. The glass body can be shaped like a test tube, with a closed bottom, which can be circular or flat. With a diameter of, for example, 3-5 mm, it can hold between 500 and

[0034] 35 x 1000 mm long.

[0035] SSY-POl-WO The hollow glass body is inserted into the process chamber in such a way that it passes through the melting zone and that the open end extends from the melting zone through the feedthrough and terminates with its opening in the filling chamber. The closed body is at least partially located in the process chamber.

[0036] 5. The feedthrough is sealed pressure-tight against the glass body. The feedthrough is then pressure-tight sealed to the end of the glass body, as well as to the filling chamber and the process chamber. The passage from which the closed body of the glass body protrudes is also sealed against the glass body. Any other passages are also sealed. Now both chambers are pressure-tight, both from each other and from the environment. The filling chamber is fluidically connected to the entire interior of the gas body.

[0037] The cooling chamber, filled with the coolant, is placed around the closed body of the glass hollow body. Preferably, the closed body of the glass hollow body is heated and evacuated shortly beforehand to allow moist air to escape.

[0038] Leave 15 and thereby reduce later condensation during cooling.

[0039] The filling process then takes place. For this, the filling chamber is vacuum-sealed using the vacuum pump and finally filled with the filling gas up to the desired filling pressure P1 using the pressure regulating device, whereby the filling gas expands inside the hollow glass body. Since the closed body of the hollow glass body is cooled and gas expands at

[0040] Since the gas in the chamber contracts significantly at cooler temperatures (20°C), the particle density there is much higher than in the uncooled chamber, where the temperature is approximately ambient. Depending on the pressure P1, the temperature may also be slightly higher.

[0041] The process chamber is set to the intended process pressure P2 by the pressure regulating device, which is at least 10 mbar, preferably 100 mbar, higher.

[0042] 25 is the filling pressure P1.

[0043] Once these pressure conditions are established, the melting zone in the process chamber is heated with the heating medium until the glass hollow body becomes plastic and is forced inwards by the lower internal pressure, thus locally sealing the glass hollow body and creating a sealed glass capsule.

[0044] 30 of a clean and hermetically sealed sealing point.

[0045] The filling process is now complete. The filling gas is pumped out of the filling chamber by the pressure regulating device, and the pressure equalization valves of both chambers are opened until ambient pressure is reached in both the filling chamber and the process chamber. The pressure-resistant closure at the feedthrough is then opened, and the seal at the passage is closed.

[0046] 35 is dissolved and the filled sealed glass capsule is removed from the process chamber.

[0047] SSY-POl-WO The glass capsule according to the invention is filled and gas-tight sealed and has a final pressure, i.e. a filling pressure at room temperature of at least 4,000 mbar, preferably at least 5,000 mbar or at least 7,000 mbar.

[0048] By the fact that the space around the melting zone in the inventive method is

[0049] Since the filling process takes place in a chamber that can be pressurized to a desired overpressure, the filling pressure P1 can also be set to ambient pressure (atmospheric pressure) or a higher pressure. The higher the filling pressure P1 during filling, the more filling gas will be contained in the sealed glass container. The filling pressure P1 can be 1,000, but also 1,300, 2,000, or even up to 3,500 mbar or more, with a filling pressure P1 of 1,300 or 3,500 mbar + / - 10% having proven suitable. Because most of the closed body of the glass container is additionally cooled in the cooling chamber during the filling process, final pressures of 4,600 to over 12,000 mbar are reached in the glass capsule at room temperature. The final pressure depends on the filling pressure P1 and the cooling temperature, as well as on the volume fraction of the closed body that is affected during filling.

[0050] 15. The filling process takes place in the cooling chamber. The melting zone should therefore be as close to the cooling chamber as possible. The luminosity of GTLS capsules, or rather the energy density of the gas, increases with higher final pressure.

[0051] It remains important with this method that the pressure in the melting zone is higher than in the inner glass tube when the melting zone is heated and the hermetic seal is created.

[0052] The pressure relief valve is created by forcing the plasticized glass inwards. This is the only way to ensure that no filling gases escape, which could potentially ignite and cause an explosion and / or the release of harmful gases.

[0053] Even without cooling, the advantage of the inventive method remains.

[0054] 25 and thus the process chamber in that the cooling chamber and in particular the liquid nitrogen can be dispensed with, which simplifies the process and makes it more cost-effective, while at the same time achieving a high final pressure in the glass capsule.

[0055] Additionally, cooling makes it possible to achieve much higher final pressures and thus transfer significantly more energy into the glass capsule. The limits are defined by

[0056] The glass thickness of the hollow glass body is set at 30, as it must not shatter. Borosilicate glass, quartz glass, sodalime glass, aluminum silicate glass, or any other type of glass can be used.

[0057] As an additional safety measure, the entire process chamber can be enclosed in a safety chamber that contains any gases released in the event of an incident.

[0058] 35 catches.

[0059] SSY-POl-WO The advantage of this method compared to similar state-of-the-art methods lies in its process reliability. The process is controlled via the set pressures P1 and P2 in the two chambers. In other methods, after setting P1, the filling chamber is additionally heated, which increases the pressure P1 but not P2. Thus

[0060] 5. The pressure P1 in the filling chamber can eventually exceed the pressure P2 in the process chamber, which can be very dangerous with the gases used here, as it risks the weld bursting, which must be absolutely avoided with these gases. In the inventive method, the closed body of the hollow glass body is cooled first, before P1 and finally P2 are set.

[0061] 10. Subsequently, heat is introduced locally in the melting zone of the process chamber to achieve sealing. This tends to increase the pressure P2, which improves process reliability. However, the filling chamber is not heated after filling in order to maintain a stable filling pressure P1. Sealing takes place at the set filling pressure P1.

[0062] 15 Brief description of the drawings

[0063] The invention is illustrated in the following drawings and explained in more detail with the aid of the reference numerals explained later. The drawings show:

[0064] Fig. 1 A schematic representation of a simple process chamber;

[0065] Fig. 2 A schematic representation of a preferred process chamber with cooling space;

[0066] 20 Fig. 3a A schematic representation of an empty trial chamber;

[0067] Fig. 3b A schematic representation of a process chamber with seals;

[0068] Fig. 4 A schematic representation according to Fig. 2 for several hollow glass bodies;

[0069] Fig. 5 a, b Examples of filled glass capsules.

[0070] Ways to implement the invention

[0071] Figure 1 shows a simple process chamber 10 for filling a hollow glass body 20 with an open end region 21 and a closed body 22, which, in use, is to be filled with a filling gas 23 consisting, at standard conditions (1 bar, 20°C), of at least 50 vol% tritium, deuterium and / or protium, and sealed gas-tight to form a glass capsule 25. These filling gases 23 are radioactive or

[0072] There are 30 explosive hazardous materials, making their handling very challenging. Radioactive gases such as tritium must never be released into the environment, not even in small quantities. Explosive substances like deuterium and protium can cause serious injuries to people nearby if they explode.

[0073] SSY-POl-WO can cause significant damage to the equipment. Since heat is used to seal the glass capsules, process safety is subject to stringent requirements.

[0074] Examples of such glass capsules 25 are shown in Figs. 5a and 5b. In these embodiments, the open end region 21 is still attached to the glass capsule 25, directly adjoining it.

[0075] 5 a sealing point 26. It is removed after the process is complete. In the production of GTLS capsules, a filling gas 23 with a tritium content of at least 80, 90 or 95% is used.

[0076] Process chamber 10 has a filling chamber 11 and a process chamber 12, which are each gas-tight and pressure-resistant during use, also from each other. They may share a common partition wall.

[0077] The filling chamber 11 can be connected to a vacuum pump 31a for emptying the filling chamber 11, or is connected to it during use. It can also be connected to a pressure regulating device 32a, which can be connected to a filling gas container 34a, for filling the filling chamber 11 with the filling gas 23 up to a predetermined filling pressure P1 >

[0078] 15 1,000 mbar. P1 can be higher than the ambient pressure P3. The pressure regulating device 32a also serves to extract residual filling gas 23 from the filling chamber 11. This can be returned to the filling gas container 34a or to another container. The filling chamber 11 can also be connected to a pressure equalization valve 33a in order to restore ambient pressure P3 in the filling chamber 11 when it is empty.

[0079] 20 According to the invention, the process chamber 12 shown in the figures has a pressure-tight sealable passage 13b, shown in Figs. 2 and 4, or an opening 14a with a pressure-tight sealable cover 14b, shown in Figs. 1 and 3a, b, for the partial or complete introduction of a hollow glass body 20 into the process chamber 12. It is also equipped with a pressure regulating device 32b for achieving a predetermined pressure.

[0080] The process pressure P2 in process chamber 12, which is higher than the filling pressure P1, can be connected via a pressure equalization valve 33b to achieve ambient pressure P3 in process chamber 12. In this simple design, the pressure control device 32b and the pressure equalization valve 33b can be integrated into a single component. In operation, they are connected to process chamber 12.

[0081] 30 Between the filling chamber 11 and the process chamber 12, a pressure-tight sealable passage 13a is formed for passing an open end region 21 of the glass hollow body 20 from the process chamber 12 into the filling chamber 11. In addition, the process chamber 12 has a melting zone 16 with a heating medium 17 for locally heating a glass hollow body 20 that passes through this melting zone 16 during use.

[0082] 35 up to its local plastic deformability.

[0083] SSY-POl-WO The process chamber 10 serves the method for filling a described glass hollow body 20 with the described filling gas 23, and for gas-tight sealing of the glass hollow body 20 to form a glass capsule 25.

[0084] As shown in Figures 2 and 4, the process space according to the invention has 12

[0085] 5 also has a pressure-tight sealable passage 13b, from which the closed body 22 of the glass hollow body 20 protrudes during use. Furthermore, the process chamber 10 additionally has a cooling chamber 40 for enclosing and cooling a closed body 22 of the glass hollow body 20 protruding from the process chamber 12, wherein the cooling chamber 40 is filled with a coolant 41, preferably liquid nitrogen, and cooled to 77 K during use. The cooling chamber 40 is well thermally insulated and preferably has a mirrored interior, as is known from Dewar flasks. The coolant 41 in the cooling chamber 40, for example the liquid nitrogen, is preferably in direct contact with the glass hollow body 20 during use to achieve optimal cooling. The glass hollow body 20 is thus immersed directly in the liquid nitrogen.

[0086] 15 immersed.

[0087] Passage 13b can be sealed to the glass body 20 in the same way as passage 13a. If no cooling is required, the cover 14b can alternatively be sealed pressure-tight against opening 14a.

[0088] Only a small area of ​​the glass hollow body 20 on both sides of the melting zone 16

[0089] 20 is located in process chamber 12. This entire area of ​​the glass hollow body 20, including the area in the feedthrough 13a and in the passage 13b, is preferably designed as a circular cylindrical glass tube, optionally also the entire closed body of the glass hollow body 22. This simple shape enables good sealing and is simple and cost-effective.

[0090] 25. Since process chamber 12 only needs to provide space for the melting zone 16, it can have a very low profile. In the figures, it is shown with a greater profile only for better illustration of the connections 31b, 33b, 18, 32b.

[0091] The process comprises the following steps: The hollow glass body 20 is placed in the process chamber 10 in such a way that it passes through the melting zone 16, whereby the

[0092] The open end region 21 from the melting zone 16 passes through the passage 13a and ends in the filling chamber 11. The closed body 22 is then either completely in the process chamber 12, as shown in Fig. 1, or protrudes from the process chamber 12 through the passage 13b, as can be seen in Figures 2 and 4.

[0093] In this position of the glass hollow body 20, the feedthrough 13a and the

[0094] 35. Passage 13b is sealed pressure-tight against the glass hollow body. Filling chamber 11 and process chamber 12 are now both gas-tight.

[0095] SSY-POl-WO The closed body 22 of the glass hollow body 20 is immersed in the cooling chamber 40. Preferably, it is heated and evacuated shortly before immersion in the coolant 41 in order to allow moist air to escape and to reduce condensation of the moist air during cooling.

[0096] 5 In use, the part of the gas-filled hollow body 20 located in the cooling chamber 40 is cooled, while the filling gas 23 expands inside the glass hollow body 20 up to the filling pressure P1, before the glass hollow body 20 is plastically sealed in the region of the melting zone 16. As the filling gas 23 cools, its volume decreases at the given pressure P1, which is equivalent to compression.

[0097] 10 According to the gas pressure equation pV=nRT (pressure px volume V = amount of substance n x gas constant R x absolute temperature T) or n=(pV) / (RT), cooling from approximately 290-300 K to 77-80 K results in a factor of 3.5 to 4 of the amount of substance n, i.e., about 3.8, depending on what percentage of the filling gas 23 can be cooled within the subsequent glass capsule 25. If, in addition, the filling pressure P1 is increased to approximately 1,300 mbar instead of 1,000 mbar, the amount of substance n in the glass capsule 25 increases by a further 30%. Overall, with the given values ​​for p and T, the amount of substance n increases by a factor of approximately 5. The final pressure in the glass capsule 25 at room temperature is therefore approximately 5,000 mbar.

[0098] For example, with a glass capsule 25 typically having a length of 770 mm, an area with a length of 736 mm can be cooled, which represents 95.5% of the volume inside the glass capsule 25.

[0099] It is noted here that the process chamber has a gas-tight sealable opening.

[0100] 10 must be implicitly present for the insertion and removal of the glass hollow body 20. Possibilities for covering 14b to the process chamber 12 and the passage 13b are shown here.

[0101] 25 described and illustrated. Other variants include such a cover for the filling chamber.

[0102] 11 or an opening mechanism for the entire process chamber 10, such as a refrigerator door, which simultaneously provides access to the filling chamber 11 and the process chamber 12, with a corresponding circumferential and central gas-tight seal. This simplifies handling the glass hollow body 20, but increases the requirements for

[0103] 30 the seals. Subsequently, these or other accessibility options will not be explicitly discussed.

[0104] For the filling process, the filling chamber 11 is first vacuum-sealed using the vacuum pump 31a and finally filled with the filling gas 23 using the pressure regulating device 32a, which is fluidically connected to a filling gas container 34a in use, until the desired pressure is reached.

[0105] 35 Filling pressure P1 filled. The filling gas 23 spreads in the filling chamber 11 as well as in the interior of the glass hollow body 20.

[0106] SSY-POl-WO The filling pressure P1 can be between 1,000 mbar and 3,500 mbar. With suitable glass, it can also be higher, up to 5,000 or even 7,000 mbar. The process gas 35 in process chamber 12 is brought below the intended process pressure P2 by the pressure regulating device 32b, which is at least 10 mbar higher than the filling pressure P1.

[0107] 5 Preferably, it is about 100 mbar or up to 200 mbar higher than the filling pressure P1. Ambient air or nitrogen can be used as the process gas 35, or a noble gas, for example helium, neon, argon or xenon.

[0108] It is emphasized here that the order in which the two pressures P1 and P2 are set up in chambers 11 and 12 is not prescribed. Chambers 11 and 12 can also be set up simultaneously with pressures P1 and P2. However, safety is increased if process chamber 12 is pressurized first, followed by filling chamber 11. Should passage 13a have a leak, filling gas would never enter the process chamber.

[0109] The closed body 22 of the glass hollow body 20 can be placed in the cooling chamber 40 cooled with the coolant 41 if the filling chamber 11 is already vacuum-sealed but

[0110] 15 is not yet filled. This further reduces condensation in the glass hollow body 20.

[0111] Once both pressures P1 and P2 are established in the two rooms 11 and 12, and the cooling chamber 40 cools the closed body 22 of the glass hollow body 20, the process for sealing the glass hollow body 20 can begin. The heating medium 17 is used to...

[0112] 20 Melting zone 16 in process chamber 12 is heated until the glass hollow body 20, which traverses the melting zone 16, has become plastic there. Due to the lower internal pressure P1 in the glass hollow body 20, it is pressed inwards in the plasticized area, thus creating the sealing point 26. This locally seals the glass hollow body 20 to create a glass capsule 25. At the sealing point 26, see Fig. 5a, 5b,

[0113] 25 of the glass hollow bodies 20 are now hermetically sealed.

[0114] In particular, the heating medium 17 can comprise a heating wire, a gas flame, or a laser. A heating wire is visualized in each of the figures. A power supply 18 can feed the respective heating medium 17 with electricity or gas. The process chamber 12 can therefore accommodate electrical and / or other feedthroughs such as a

[0115] 30 gas lines, as shown for the heating medium 17. A laser can be used without feedthroughs. Further feedthroughs, not shown, may be provided in the filling chamber 11 and in the process chamber 12, for example for the installation of pressure and / or temperature sensors. Lines 30 as flow-related connections are provided accordingly to all pressure regulating devices 32 and vacuum pumps 31.

[0116] 35 and pressure equalization valves 33 are provided.

[0117] To complete the process, the glass capsule 25 must be removed from the process chamber 10. For this purpose, the filling gas 23 is first pumped out of the filling chamber 11 using the pressure regulating device 32a and returned to the filling gas container 34a or another container. The pressure equalization valves 33a, b are then

[0118] 5 is opened until ambient pressure P3 is restored in filling chamber 11 and process chamber 12. In this state, feedthrough 13a and passage 13b or cover 14b can be reopened. The glass capsule 25 can now be removed from process chamber 10.

[0119] Figure 2 shows the inventive variant of the process chamber 12. The state after melting is also shown, with the sealing point 26 in the area of ​​the melting zone 16 and the sealed glass capsule 25.

[0120] It is also possible to achieve higher filling pressures P1, for example up to 2000 mbar, up to 2500 mbar, up to 3000 mbar, or up to 3500 bar. Limits are imposed by the glass of the hollow glass body 20, which must withstand the corresponding pressure P1 without cracking.

[0121] Break 15. With a filling pressure P1 of 3,500 mbar, a final pressure of over 13,000 mbar can be achieved in the glass capsule 25.

[0122] The high filling pressure P1 is made possible according to the invention by carrying out the melting process in process chamber 12 under an adjustable pressure P2, which is always higher than P1. This ensures the safety required when handling the gases mentioned.

[0123] 20 In addition, the rooms themselves offer further safety by being able to collect the gases should an error occur during the melting process.

[0124] In another preferred embodiment, also shown in Fig. 2, the process chamber 12 can be connected to a vacuum pump 31b for emptying the process chamber 12. The pressure control device 32b of the process chamber 12 is then connected to a

[0125] 25 process gas containers 34b are connectable for filling the process chamber 12 with a process gas 35 from the process gas container 34b and for returning the process gas 35, preferably back into the process gas container 34b. Argon, for example, can be used as the process gas.

[0126] In use, the process chamber 12 is pre-treated with the process pressure P2.

[0127] The vacuum pump 31b is emptied and then filled with the process gas 35. After sealing in the melting zone 16, the process gas 35 is pumped out of the process chamber 12 again by the pressure regulating device 32b, preferably back into the process gas container 34b, before the pressure equalization valve 33b is opened. Here, too, the devices for pressures P1, P2, as well as the subsequent emptying and

[0128] 35 The subsequent pressure equalization to the ambient pressure P3 is carried out simultaneously.

[0129] SSY-POl-WO will be, or one after the other, since rooms 11 and 12 are independent of each other in terms of printing technology.

[0130] The device according to Fig. 1 can also be equipped with a connection to a process gas container 34b, as shown in Fig. 2, and / or with a cooling chamber 40,

[0131] 5 which surrounds the lens- or spherical closed body 22.

[0132] A seal 15 may be fitted at the passage 13a, at the passage 14b, between the opening 14a and the cover 14b and / or at any other opening to the process chamber 10, which is preferably made of rubber, metal, plastic or stone fiber.

[0133] 10 The filling chamber 11 and the process chamber 12 can be designed as two separate, movable chambers, as shown in Figures 3a and 3b, or as one chamber with a common partition wall with the feedthrough 13a, as shown in Figures 1 and 2. They can preferably be made of metal, composite materials, fiber material, glass, sapphire, acrylic glass, plastic or a mixture thereof.

[0134] 15 In the embodiment shown in Figures 3a and 3b, the filling chamber 11 and the process chamber 12 form two completely separate chambers that are independent of each other, with at least one seal 15 arranged at the opening 13a between the filling chamber 11 and the process chamber 12, and preferably another seal 15 between the process chamber 12 and either the cover plate 14b, as shown here, or the cooling chamber 40. Furthermore, this process chamber 10, as shown in Figure 3b, includes a force device 19 which, in use, can exert a force from the outside on the filling chamber 11 in the direction of the process chamber 12, so that these two chambers 11, 12 are pressed against each other.

[0135] In use, after the glass hollow body 20 is inserted into the process chamber 10

[0136] 25 according to Fig. 3 a and b, at least the passage 13a, preferably also the passage 13b, or the opening 14a with the cover 14b, is sealed pressure-tight and gas-tight by means of the force device 19, exerting a force from the outside on the filling chamber 11 in the direction of the process chamber 12, as shown by arrows in Fig. 3b. This seals at least the seal 15 between the filling chamber 11 and the process chamber 12 on the filling chamber 11, on the

[0137] 30 Process chamber 12 and at the open end area of ​​the glass hollow body 21 are sealed gas-tight and pressure-resistant.

[0138] The same applies to the further seal 15 between the process chamber 12 and either the cover plate 14b or at the passage 14 to the cooling chamber 40. As soon as the force is released again by the force device 19, the glass hollow body 20 is also

[0139] 35 has been released and can be removed.

[0140] Alternatively, an adapter (not shown) can be used as a seal, which is first applied, screwed or welded onto the glass hollow body 20, the filling chamber 11 or the process chamber 12.

[0141] Preferably, the process chamber 10 comprises a control unit 50, with which the

[0142] 5. The filling, emptying, and / or setting of the predefined pressures P1 and P2 in the filling chamber 11 and / or in the process chamber 12 is controlled. It can preferably also control or regulate the heat input of the heating medium 17. However, the control can also be performed manually by a user.

[0143] As shown in Fig. 4, the process chamber 10 can have two or more feedthroughs 13a and melting zones 16 with heating elements 17 for simultaneously filling and sealing two or more hollow glass bodies 20. The heating element 17 shown schematically is a heating wire that heats all melting zones 16. Preferably, individual heating wires would be arranged as heating elements 17 for each melting zone 16 so that they can be replaced more easily in case of a defect. With multiple feedthroughs 13a

[0144] 15 These are preferably all arranged in a row. This simplifies the handling and placement of the heating elements 17, especially if each melting zone 16 comprises its own heating element 17, for example a laser or a heating wire.

[0145] It is emphasized here that filling chamber 11 is not heated for safety reasons, because this would increase the filling pressure P1 in filling chamber 11 and thus endanger process safety.

[0146] 20 would. For the same reason, process chamber 12 is also not cooled: the process pressure P2 would decrease. Heating process chamber 12 with the heating medium 17 for the melting process increases process reliability.

[0147] The glass hollow bodies 20 can be internally coated and / or have one or more inserts 24 that were previously introduced, as shown in Figures 1, 2 and 4.

[0148] 25 shown.

[0149] Following the filling and finishing of the glass capsules 25 according to the invention, they can be divided into smaller portions in further processes. A process chamber 10 can again be used for this purpose to adjust the pressure in the process chamber 12 accordingly. Furthermore, a sealing point can also be created by heating.

[0150] 30 twisting and / or mechanical impact such as crushing can be achieved.

[0151] The glass capsule 25 according to the invention is filled and sealed with a filling gas 23 consisting of at least 50 vol% tritium, deuterium and / or protium under standard conditions. It has a filling pressure at room temperature of at least 4,000 mbar, or at least 5,000 or 10,000 mbar, wherein the glass capsule 25 has exactly one sealing point 26.

[0152] 35. Following the seal point 26, it is designed in a circular cylindrical shape.

[0153] The SSY-POl-WO glass capsule 25 can be, in particular, a GTLS, a TGLQ (Tritium Gas Light Source), or a battery. It can be designed as a cylindrical rod or lens-shaped.

[0154] One advantage of this process chamber 10 is that the cooling room 40 and the process chamber 12 are separate from each other. The cooling room 40 is located outside the

[0155] 5 Process room 12. Thus, the cooling does not lower the temperature in process room 12 and the process is safer overall.

[0156] Reference symbol list

[0157] 10th Trial Chamber

[0158] 11 Filling chamber

[0159] 10 12 Process room

[0160] 13 a: Pressure-tight feedthrough; b: Pressure-resistant passage

[0161] 14 a: Opening b: Cover

[0162] 15 Seal

[0163] 16 Melting zone

[0164] 15 17 Heating fuel

[0165] 18 Energy supply

[0166] 19 Power unit

[0167] 20 glass hollow bodies

[0168] 21 Open end region of the gas cavity

[0169] 22 Closed body of the gas cavity

[0170] 23 Filling gas

[0171] 24 Insert or coating in the closed body of the glass hollow body

[0172] 25 filled glass containers; sealed glass capsules

[0173] 26 Sealing station

[0174] 25 30 a, b line

[0175] 31 a, b vacuum pump

[0176] 32 a, b Pressure regulating device

[0177] 33 a, b Pressure equalization valve

[0178] 34 a: Filling gas container, b: Process gas container

[0179] 30 35 Process gas

[0180] 40 Cold storage room

[0181] 41 Coolant

[0182] 50 Control

[0183] P1 Filling pressure

[0184] 35 P2 process pressure

[0185] P3 Ambient pressure

[0186] SSY-POl-WO

Claims

Patent claims 1. Process chamber (10) for filling and sealing a glass hollow body (20) with an open end region (21) and a closed body (22), which in use with a filling gas (23) consisting of a standard gas (1 bar, 20°C) 5. The process chamber (10) is to be filled with at least 50 vol% tritium, deuterium and / or protium and sealed gas-tight, wherein the process chamber (10) has a filling chamber (11) and a process chamber (12), each of which is sealed gas-tight and pressure-resistant in use, wherein 10 the filling chamber (11) with a vacuum pump (31a) for emptying the filling chamber (11) is connectable and is connectable via a pressure regulating device (32a) to a filling gas container (34a) for filling the filling chamber (11) with a filling gas (23) up to a predetermined filling pressure (P1) of > 1,000 mbar and for removing residual filling gas (23) from the filling chamber (11), preferably for its return to the filling gas container (34a), and is connectable to a pressure equalization valve (33a) to achieve ambient pressure (P3) in the emptied filling chamber (11); and the process chamber (12) is connectable to a pressure regulating device (32b) suitable for achieving a predetermined process pressure (P2) in the process chamber (12), which is higher than the filling pressure (P1), and can be connected to a pressure equalization valve (33b) to achieve ambient pressure (P3) in the process chamber (12), and a pressure-tight sealable passage (13a) is formed between the filling chamber (11) and the process chamber (12) for passing an open end region (21) of the glass hollow body (20) from the process chamber (12) into the 25 Filling chamber (11), and wherein the process chamber (12) has a melting zone (16) with a heating medium (17) in which a glass hollow body (20) can be locally heated until it reaches its plastic deformability, characterized in that 30 the process chamber (12) has a pressure-tight sealable passage (13b) from which, in use, the closed body (22) of the gas hollow body (20) protrudes, and the process chamber (10) additionally has a cooling chamber (40) for enclosing and cooling a gas hollow body (20) protruding from the process chamber (12). 35 closed body (22) of the glass hollow body (20), wherein the cooling chamber (40) is preferably suitable for being cooled with liquid nitrogen during use. -POl-WO 2. Process chamber according to claim 1, characterized in that the filling chamber (11) is connected to the vacuum pump (31a), the pressure regulating device (32a) and to the pressure equalization valve (33a).

3. Trial chamber according to one of the preceding claims, thereby 5 characterized in that the process chamber (12) is connected to a vacuum pump (31 b) for emptying the process chamber (12), and to the pressure regulating device (32b), which can be connected to a process gas container (34b), for filling the process chamber (12) with a process gas (35) from the process gas container (34b) and preferably for returning the process gas (35) to the process gas container (34b), and to the pressure equalization valve (33b).

4. Process chamber according to one of the preceding claims, wherein the filling chamber (11) and the process chamber (12) form two separate chambers which are movable relative to each other, and wherein at least one seal (15) is arranged at the passage (13a) between the filling chamber (11) and the process chamber (12), 15 comprising a force device (19) which, in use, can exert a force from the outside on the filling chamber (11) in the direction of the process chamber (12), whereby the seal (15) can seal gas-tight and pressure-resistant during the passage (13a) by this force on the filling chamber (11), on the process chamber (12) and on the open end area of ​​the glass hollow body (21). 20 5. Process chamber according to one of the preceding claims, characterized by a control (50) for controlling the filling, emptying and / or the setting of the predetermined pressures (P1 , P2) in the filling chamber (11) and / or in the process chamber (12) and preferably for controlling or regulating the heat input of the heating medium 17. 25 6. Process chamber according to one of the preceding claims, characterized by two or more feedthroughs (13a), passages (13b) and melting zones (16) for the simultaneous filling of two or more glass hollow bodies (20).

7. Method for filling and sealing a glass hollow body (20) with a filling gas (23) consisting of at least 50 vol% tritium, deuterium and / or protium at 30 Standard conditions for a glass capsule (25) using a process chamber (10) according to one of the preceding claims and a glass hollow body (20) with a closed body (22) and an open end region (21) for filling, characterized in that the glass hollow body (20) is introduced into the process chamber (10) in such a manner, 35 that it crosses the melting zone (16) and that the open end region (21) crosses the passage (13a) from the melting zone (16) and im-POl-WO The filling chamber (11) ends, with the closed body (22) being at least partially in the process chamber (12); - wherein the closed body (22) of the gas hollow body (20) passes through the passage (13b), protrudes from the process chamber (12) and from the cooling chamber (40) 5 is enclosed and cooled so that the feedthrough (13a) and the passage (13b) against the glass hollow body (20) are pressure-tested and sealed until the filling chamber (11) and the process chamber (12) are gas-tight and pressure-tested, the filling chamber (11) is vacuum-sealed with the vacuum pump (31a) and finally with 10 of the pressure regulating device (32a) is filled with the filling gas (23) up to the desired filling pressure (P1) > 1,000 mbar, whereby the filling gas (23) spreads inside the glass hollow body (20), the process chamber (12) with the pressure regulating device (32b) is set under the intended process pressure (P2), which is at least 10 mbar, preferably 100 mbar, greater than the filling pressure (P1), the melting zone (16) in the process chamber (12) is heated with the heating medium (17) until the glass hollow body (20) has become plastic in the area of ​​the melting zone (16) and is pushed inwards by the lower internal pressure P1 in the glass hollow body (20) and the glass hollow body (20) is thereby locally sealed, to create a glass capsule (25) which is closed at a sealing point (26), - wherein the closed body (22) of the gas hollow body (20) is cooled in the cooling chamber (40), while the filling gas (23) spreads inside the glass hollow body (20) until the glass hollow body (20) is in the area of ​​the melting zone (16) 25 is plastically sealed, the filling gas (23) is pumped out of the filling chamber (11) again with the pressure regulating device (32a), the pressure equalization valves (33a, b) are opened until ambient pressure (P3) is reached in the filling chamber (11) and in the process chamber (12), 30 the passage (13a) and the passage (13b) are reopened, and the glass capsule (25) is removed from the process chamber (10).

8. Method according to claim 7, characterized in that the filling pressure (P1) is between 1,300-3,500 mbar or up to 5,000 mbar and the process pressure (P2) is between 10 and 200 mbar, preferably 100 mbar higher than the filling pressure (P1). 35 9. Method according to claim 7 or 8 using a process chamber (10) according to claim 3, characterized in that the process space (12) is located before the -POl-WO The process pressure (P2) is applied by the vacuum pump (31 b) and the process chamber (12) is then emptied and subsequently filled with a process gas (35), for example argon, which is pumped out of the process chamber (12) again by the pressure control device (32b) before the pressure equalization valve (33b) is opened. 5 10. Method according to one of claims 7 to 9, characterized in that the closed body (22) of the gas hollow body (20) is heated and evacuated before it is enclosed and cooled by the cooling chamber (40) in order to reduce condensation.

11. Method according to one of claims 7 to 10, characterized in that one or more inserts (24) are placed in the closed body (22) or an inner coating is applied.

12. Method according to one of claims 7 to 11 and using a process chamber (10) according to claim 4, characterized in that after the glass hollow body (20) has been placed in the process chamber (10) the following is carried out 15 (13a) is sealed in a pressure-tight and gas-tight manner by applying a force from the outside to the filling chamber (11) in the direction of the process chamber (12) by means of the force device (19), whereby the seal (15) between the filling chamber (11) and the process chamber (12) seals gas-tight and pressure-tight at the filling chamber (11), at the process chamber (12) and at the open end area of ​​the glass hollow body (21) by means of this force. 20 13. Method according to one of claims 7 to 12 and using a process chamber (10) according to claim 5, characterized in that the control unit (50) controls the filling, emptying and / or the setting of the predetermined pressures (P1, P2) in the filling chamber (11) and / or in the process chamber (12) and preferably controls or regulates the heat input of the heating medium (17). 25 will be.

14. Method according to one of claims 7 to 13 and using a process chamber (10) according to claim 6, characterized in that two or more glass hollow bodies (20) are introduced into the process chamber (10) and thus two or more glass hollow bodies (20) are filled and sealed simultaneously. 30 15. Glass capsule (25), filled with a filling gas (23) of at least 50 vol% tritium, deuterium and / or protium under standard conditions and sealed according to a method of claims 7 to 14, characterized by a filling pressure at room temperature of at least 4,000 mbar, or of at least 5,000 mbar, wherein the glass capsule (25) has exactly one sealing point (26) and the area 35 next to the seal (16) is designed in a circular cylindrical shape. -POl-WO

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